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Rapid evaluation of edible hemp oil quality using NMR and FT-IR spectroscopy
Abstract
Since Cannabis species include psychoactive varieties containing high levels of Δ9-tetrahydrocannabinol (THC), psychotropic properties could be wrongly attributed to hemp-seed oil obtained from Cannabis sativa. Hemp oil does not exert any psychotic effect; on the contrary, it may provide significant health benefits, because it has an optimum proportion of ω-6 to ω-3 fatty acids (3:1). Six samples of cold pressed hemp-seed oils were studied by nuclear magnetic resonance (NMR) and Fourier-transformed infrared spectroscopy (FT-IR). These methods were applied to evaluate the ratio of ω-6 to ω-3 fatty acids, to control the origin, composition and presence of adulteration in hemp oils. FT-IR method allowed us to distinguish three oils with the highest level of γ-linolenic acid. Additionally, NMR spectroscopy was applied to determine the ω-6 to ω-3 ratio. The outcomes of the NMR experiment are in agreement with GC outcomes measures. The results indicate that NMR and FT-IR may be used in routine evaluation of hemp-seed oil quality as a fast and reliable method of verification of ω-6 to ω-3 ratio and origin of the oil.
... From these extracts, 1D 1 H NMR spectra were recorded to be used for reproducibility and standard deviation in the calculation of the essential fatty acids ratio. 1 H NMR spectra were manually phased, baseline-corrected, and the chemical shifts were reported with respect to the TMS signal used as reference. From the 1 H NMR spectra of these extracts, the main fatty acids ω-6/ω-3 ratio can be determined by combining the integrals, obtained after applying the deconvolution procedure, of three different signals: (a) the methyl protons of all the acyl groups (LA), with the exception of those of α-linolenic acid; (b) the methyl protons of ω-3 fatty acid (α-linolenic acid (αLA)); (c) the methylene protons of the linoleic and α-linolenic acyl groups; and using the relations [38]: ...
... ppm generated by the diallylic protons of the linoleic and α-linolenic acyl groups. By combining the area of these signals, using the relations (1) and (2) that take into account the number of equivalent nuclei in each group, the concentrations of αLA and LA were calculated, from which the ω-6/ω-3 ratio was obtained [38]. ...
... Indeed, the measurement of this ratio is based only on the recording and analysis of the 1 H NMR spectra obtained directly from the seed extracts without further derivatization, as is required by the gas chromatography (GC) method, the common and validated method used to determine the composition of oil in terms of fatty acids [56]. Moreover, our result agrees with that reported in the paper of Siudem et al. [38] in which the authors analyzed six different samples of hemp seed oils and calculated the ω-6/ω-3 ratio by 1 H NMR for each of them using the relationships (1) and (2). The authors compared these data with those from CG method applied to the same hemp seed oils and found a substantial agreement between them, which proves the effectiveness of the method. ...
Cannabis sativa is a herbaceous multiple-use species commonly employed to produce fiber, oil, and medicine. It is now becoming popular for the high nutritional properties of its seed oil and for the pharmacological activity of its cannabinoid fraction in inflorescences. The present study aims to apply nuclear magnetic resonance (NMR) spectroscopy to provide useful qualitative and quantitative information on the chemical composition of seed and flower Cannabis extracts obtained by ultra-sound-assisted extraction, and to evaluate NMR as an alternative to the official procedure for the quantification of cannabinoids. The estimation of the optimal ω-6/ω-3 ratio from the 1H NMR spectrum for the seed extracts of the Futura 75 variety and the quantitative results from the 1H and 13C NMR spectra for the inflorescence extracts of the Tiborszallasi and Kompolti varieties demonstrate that NMR technology represents a good alternative to classical chromatography, supplying sufficiently precise, sensitive, rapid, and informative data without any sample pre-treatment. In addition, different extraction procedures were tested and evaluated to compare the elaboration of spectral data with the principal component analysis (PCA) statistical method and the quantitative NMR results: the extracts obtained with higher polarity solvents (acetone or ethanol) were poor in psychotropic agents (THC < LOD) but had an appreciable percentage of both cannabinoids and triacylgliceroles (TAGs). These bioactive-rich extracts could be used in the food and pharmaceutical industries, opening new pathways for the production of functional foods and supplements.
... This work This work This work This work This work This work Ref. [28] This work Ref. [21] Ref. [23] Ref. [24] Tentative IR band assignments [24] Ref. [25] Tentative Raman band assignments [25] Ref. [22] Tentative IR band assignments [ The description and assignment of the IR spectra was conducted following the available literature with an emphasis of the analytical bands responsible for differentiation of the cannabinoids of our interest: THCA, THC, CBDA, and CBD (Fig. 1). Firstly, given the need for precise spectral examination, two air-dried, non-thermally treated flowers (FL1 and FL2) were screened ( Table 1). ...
... This work This work This work This work This work This work Ref. [28] This work Ref. [21] Ref. [23] Ref. [24] Tentative IR band assignments [24] Ref. [25] Tentative Raman band assignments [25] Ref. [22] Tentative IR band assignments [ The description and assignment of the IR spectra was conducted following the available literature with an emphasis of the analytical bands responsible for differentiation of the cannabinoids of our interest: THCA, THC, CBDA, and CBD (Fig. 1). Firstly, given the need for precise spectral examination, two air-dried, non-thermally treated flowers (FL1 and FL2) were screened ( Table 1). ...
... [24] Tentative IR band assignments [24] Ref. [25] Tentative Raman band assignments [25] Ref. [ tion next to the carboxylic group around 1180 cm À1 . However, the most intense absorption around 1250 cm À1 , slightly shifted among the THCA and CBDA spectra, is ascribed to the m(C-OH) vibration from the carboxylic group since upon decarboxylation the intensity of this band majorly decreases (see forthcoming discussion). ...
Tetrahydrocannabinol (THC) and cannabidiol (CBD) are the most notable Cannabis components with pharmacological activity and their content in the plant flowers and extracts are considered as critical quality parameters. The new Medical Cannabis industry needs to adopt the quality standards of the pharmaceutical industry, however, the variability of phytocannabinoids content in the plant material often exerts an issue in the inconsistency of the finished product quality parameters. Sampling problems and sample representativeness is a major limitation in the end-point testing, particularly when the expected variation of the product quality parameters is high. Therefore, there is an obvious need for the introduction of Process Analytical Technology (PAT) for continuous monitoring of the critical quality parameters throughout the production processes. Infrared spectroscopy is a promising analytical technique that is consistent with the PAT requirements and its implementation depends on the advances in instrumentation and chemometrics that will facilitate the qualitative and quantitative aspects of the technique. Our present work aims in highlighting the potential of mid-infrared (MIR) spectroscopy as PAT in the quantification of the main phytocannabinoids (THC and CBD), considered as critical quality/material parameters in the production of Cannabis plant and extract. A detailed assignment of the bands related to the molecules of interest (THC, CBD) was performed and the spectral features of the decarboxylation of native flowers were identified, and the acid forms (THCA, CBDA) specific bands were assigned and thoroughly explained. Further, multivariate models were constructed for the prediction of both THC and CBD content in extract and flower samples from various origins, and their prediction ability was tested on a separate sample set. Savitskzy-Golay smoothing and the second derivative of the native MIR spectra (1800-400 cm⁻¹ region) resulted in best-fit parameters. The PLS models presented satisfactory R2Y and RMSEP of 0.95 and 3.79% for THC, 0.99 and 1.44% for CBD in the Cannabis extract samples, respectively. Similar statistical indicators were noted for the Partial least-squares (PLS) models for THC and CBD prediction of decarboxylated Cannabis flowers (R2Y and RMSEP were 0.99 and 2.32% for THC, 0.99 and 1.33% for CBD respectively). The VIP plots of all models demonstrated that the THC and CBD distinctive band regions bared the highest importance for predicting the content of the molecules of interest in the respected PLS models. The complexity of the sample (plant tissue or plant extract), the variability of the samples regarding their origin and horticultural maturity, as well as the non-uniformity of the plant material and the flower-ATR crystal contact (in the case of Cannabis flowers) were governing the accuracy descriptors. Taking into account the presented results, ATR-MIR should be considered as a promising PAT tool for THC and CBD content estimation, in terms of critical material and quality parameters for Cannabis flowers and extracts.
... Health benefits of hemp seed are related to the high level of polyunsaturated fatty acids (PUFAs) present in the seed (Kolodziejczyk et al., 2012). Hemp-seed oil does not exert psychotic effect; whereas, it exhibits health beneficial activity due to its optimum proportion ofω-6 linoleic acid andω-3 alpha-linolenic acid (3:1) as recommended in healthy diet (Siudem et al., 2019;Da Porto et al., 2015). [136,137] Vitamins D and E (fat-soluble vitamins) are other important constituents in hemp-seed oil. ...
... Hemp-seed oil does not exert psychotic effect; whereas, it exhibits health beneficial activity due to its optimum proportion ofω-6 linoleic acid andω-3 alpha-linolenic acid (3:1) as recommended in healthy diet (Siudem et al., 2019;Da Porto et al., 2015). [136,137] Vitamins D and E (fat-soluble vitamins) are other important constituents in hemp-seed oil. After extraction of hemp seed oil, the residue can be converted into various protein-rich food products. ...
... The thin band, observed in the 1734 cm −1 region, indicates a possible stretch of C = O of the ester, indicating the presence of oil. The esters have two absorption regions, ranging from 1750-1730 and 1300-1000 cm −1 (Guillén and Cabo, 1997;Siudem et al., 2019). The band of medium width observed in the region of 1602 cm −1 , possibly represents a C = O connection stretch of the aldehyde, present in the sugar composition. ...
... The acute band of greater intensity, observed in the region of 1070 cm −1 , points to a probable elongation of the C = O ester bond and the highest values of oleic acid in 360 DAA (Table S1). The bands close to 700 cm −1 correspond to the CH 2 and CH vibrations (Siudem et al., 2019). The relatively small variation between the ranges is related to the sample nature, since the macauba pulp used in this study presented some interferents, such as structural and non-structural carbohydrates. ...
Macauba palm (Acrocomia aculeata (Jacq.) Lodd. ex Mart. Arecaceae) is a novel oil crop with wide industrial applicability. However, little is known about the photosynthetic responses to seasonality during fruit development in macauba palm and its effects on the fatty acid profile of mesocarp oil and its physicochemical and spectroscopic characteristics. The fatty acid profile changed in six fruit developmental stages (ranging from 180 days after anthesis to full ripening and dispersion). This occurred during the transition from dry to rainy season concomitant with adjustments in photosynthetic responses. The increase in mesocarp oil yield in the fruit was synchronized with the higher photosynthetic capacity at the beginning of the rainy season, being characterized by a raise in oleic acid. The dynamics of soluble solids, acidity, pH, total sugars and starch were proportional to the spectroscopic changes and allowed to determine the ideal harvest point: 360 days after anthesis, with fruits still in the bunch. The macauba palm fruits in this stage showed suitable physical and chemical characteristics for industrial use, as well as higher oil yield. The monitoring of chemical changes with Fournier transformed infrared spectroscopy techniques would aid fast and precise detection of the fruit development and its ideal harvest point.
... Structural formula of THCA (Fig. 1, left) infers that the carboxylic group is positioned in adjacent position to both the n-pentyl chain and the phenolic OH group. In this region, mainly the bands from the bending CH 2 and CH 3 vibrations within the n-pentyl chain (and in the cyclohexene ring) as well as one band from the CC stretchings from the aromatic ring were assigned [22,26,27] (Table 1). ...
... Here, it is worth emphasizing that the assignment of the bands were delivered in close resemblance to the scarce available literature results for cannabis and hemp samples [14,18,19,[25][26][27] and mostly relying on the very recent and detailed theoretical vibrational (infrared and Raman) properties of THC and CBD molecules [22]. ...
The decarboxylation of Δ9-tetrahydrocannabinolic acid (THCA) plays pivotal role in the potency of medical cannabis and its extracts. Our present work aims to draw attention to mid-infrared (MIR) spectroscopy to in-situ monitor and decipher the THCA decarboxylation reaction in the solid state. The initial TG/DTG curves of THCA, for a first time, outlined the solid–solid decarboxylation dynamics, defined the endpoint of the process and the temperature of the maximal conversion rate, which aided in the design of the further IR experiment. Temperature controlled IR spectroscopy experiments were performed on both THCA standard and cannabis flower by providing detailed band assignment and conducting spectra-structure correlations, based on the concept of functional groups vibrations. Moreover, a multivariate statistical analysis was employed to address the spectral regions of utmost importance for the THCA → THC interconversion process. The principal component analysis model was reduced to two PCs, where PC1 explained 94.76% and 98.21% of the total spectral variations in the THCA standard and in the plant sample, respectively. The PC1 plot score of the THCA standard, as a function of the temperature, neatly complemented to the TG/DTG curves and enabled determination of rate constants for the decarboxylation reaction undertaken on several selected temperatures. The predictive capability of MIR was further demonstrated with PLS (R2X = 0.99, R2Y = 0.994 and Q2 = 0.992) using thermally treated flower samples that covered broad range of THCA/THC content. Consequently, a progress in elucidation of kinetic models of THCA decarboxylation in terms of fitting the experimental data for both, solid state standard substance and a plant flower, was achieved. The results open the horizon to promote an appropriate process analytical technology (PAT) in the outgrowing medical cannabis industry.
... Structural formula of THCA (Fig. 1, left) infers that the carboxylic group is positioned in adjacent position to both the n-pentyl chain and the phenolic OH group. In this region, mainly the bands from the bending CH 2 and CH 3 vibrations within the n-pentyl chain (and in the cyclohexene ring) as well as one band from the CC stretchings from the aromatic ring were assigned [22,26,27] (Table 1). ...
... Here, it is worth emphasizing that the assignment of the bands were delivered in close resemblance to the scarce available literature results for cannabis and hemp samples [14,18,19,[25][26][27] and mostly relying on the very recent and detailed theoretical vibrational (infrared and Raman) properties of THC and CBD molecules [22]. ...
p>The decarboxylation of Δ9-tetrahydrocannabinolic acid (THCA) plays pivotal role in the potency of medical cannabis and its extracts. However, the literature data point out substantial variations in the process reaction rate and conversion efficacy due to variability of the temperature, heat transfer efficacy, raw material attributes, consequently resulting in incomplete decarboxylation, cannabinoid content decrease due to decomposition, evaporation, and possible side reactions. Our present work aims to draw attention to mid-infrared (MIR) spectroscopy for in-situ monitoring and decipher the THCA decarboxylation reaction in the solid state. The initial TG/DTG curves of THCA, for a first time outlined the solid-solid decarboxylation dynamics, defined the endpoint of the process and the temperature of the maximal conversion rate, which aided in the design of the further IR experiments. Temperature controlled IR spectroscopy experiments were performed on both THCA standard and cannabis flower by providing detailed band assignment and conducting spectra-structure correlations, based on the concept of functional groups vibrations. Moreover, a multivariate statistical analysis was employed to depict the spectral regions of utmost importance for the THCA→THC interconversion process. The principal component analysis model was reduced to two PCs, where PC1 explained 94.76% and 98.21% of the total spectral variations in the THCA standard and in the plant sample, respectively. The PC1 plot score of the THCA standard, as a function of the temperature, neatly complemented to the TG/DTG curve and enabled determination of rate constants for the decarboxylation reaction undertaken on several temperatures. Consequently, a progress in elucidation of kinetic models of THCA decarboxylation, fitting experimental data for both, solid state standard substance and a plant flower, was achieved. The results open the horizon to promote an appropriate process analytical technology (PAT) in the outgrowing medical cannabis industry.</p
... In order to identify the cannabinoids existing in hempseed oil samples, LC-MS analyses were carried out according to Citti et al. 18 using an Agilent 1290 Infinity/6530 Accurate Mass Q-TOF equipped with MassHunter Workstation software B.07.00. The column was Agilent Zorbax Eclipse Plus C18, 2.1 × 50 mm, with 1.8 μm pore size. ...
... The fatty acid compositions and the ratios among them were determined from the areas from the characteristic signals of each fatty acyl chain (See Supplemental Fig. 2). We confirmed former findings 18 , that at the main composition of fatty acids in HSO include linolenic acid (ω-3), linoleic acid (ω-6), oleic acid (ω-9) and saturated fatty acid. The ratio between linoleic acid (ω-6): linolenic acid (ω-3) and linolenic acid (ω-3): oleic acid (ω-9) was measured to be 3.12 and 2.16, respectively. ...
Abstract The seed of the hemp plant (Cannabis sativa L.) has been revered as a nutritional resource in Old World Cultures. This has been confirmed by contemporary science wherein hempseed oil (HSO) was found to exhibit a desirable ratio of omega-6 and omega-3 polyunsaturated fatty acids (PUFAs) considered optimal for human nutrition. HSO also contains gamma-linoleic acid (GLA) and non-psychoactive cannabinoids, which further contribute to its’ potential bioactive properties. Herein, we present the kinetics of the thermal stability of these nutraceutical compounds in HSO, in the presence of various antioxidants (e.g. butylated hydroxytoluene, alpha-tocopherol, and ascorbyl palmitate). We focussed on oxidative changes in fatty acid profile and acidic cannabinoid stability when HSO was heated at different temperatures (25 °C to 85 °C) for upto 24 h. The fatty acid composition was evaluated using both GC/MS and 1H-NMR, and the cannabinoids profile of HSO was obtained using both HPLC-UV and HPLC/MS methods. The predicted half-life (DT50) for omega-6 and omega-3 PUFAs in HSO at 25 °C was about 3 and 5 days, respectively; while that at 85 °C was about 7 and 5 hours respectively, with respective activation energies (Ea) being 54.78 ± 2.36 and 45.02 ± 2.87 kJ/mol. Analysis of the conjugated diene hydroperoxides (CDH) and p-Anisidine value (p-AV) revealed that the addition of antioxidants significantly (p
... The analysis of the authenticity of cold-pressed and refined oils usually entails a list of physical, chemical, and sensory tests. Several analytical techniques are employed for this purpose, e.g., gas chromatography (GC) [Xu et al., 2015], high-performance liquid chromatography (HPLC) [Ratusz et al., 2018], and various spectroscopy methods such as UV-visible spectroscopy [Karbasian et al., 2015], nuclear magnetic resonance (NMR) [Siudem et al., 2019], and Fourier transform infrared spectroscopy (FTIR) [Moigradean et al., 2015] being the most widely deployed. However, thermal analysis is an emerging technique that has proved useful in authenticating oil products. ...
The authenticity assessment of edible oils is crucial to reassure consumers of product compliance. In this study, a new
approach was taken to combining untargeted profiling by using differential scanning calorimetry (DSC) with chemometric
methods in order to distinguish cold-pressed oils (flaxseed, camelina, hempseed) from refined oils (rapeseed, sunflower,
soybean). The whole spectrum of DSC melting profiles was considered as a fingerprint of each oil. Flaxseed and hempseed
oils exhibited four endothermic peaks, while three peaks with one exothermic event were detected for camelina seed
oil. In the case of refined oils, two endothermic peaks were detected for rapeseed oil, three for sunflower oil and four for
soybean oil. Thermodynamic parameters, such as peak temperature, peak heat flow and enthalpy, differed for each type
of oil. Principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) were used
for processing data consisting of the whole spectrum of heat flow variables of melting phase transition. PCA demonstrated
a clear separation between refined and cold-pressed oils as well as six individual oils. The OPLS-DA showed a distinct clas�sification in six classes according to the types of oils. High OPLS-DA coefficients including R2
X(cum)=0.971, R2
(cum)=0.916
and Q2
X(cum)=0.887 indicated good fitness of the model for oil discrimination. Variables influence on projection (VIP) plot
indicated the most significant variables of the heat flow values detected at temperatures around −29°C, −32°C, −14°C,
−10°C, −24°C and −41°C for the differentiation of oils. The study ultimately demonstrated great potential of the untargeted
approach of using the whole melting DSC profile with chemometrics for the discrimination of cold-pressed and refined oils.
... In addition, the w-3/w-6 ratio is 3:1, which agrees with European Food Safety Agency recommendations [71]. Its unsaponifiable fraction is also a source of interesting minor bioactive compounds such as tocopherols, vitamins D and E, and phytosterols [45]. Linseed oil (Linum usitatissimum L.) is an important component in the development of functional foods, as it is rich in polyunsaturated fatty acids and phenolic compounds [72]. ...
In the present day, it has been widely established that a high intake of animal fat that contains a high content of saturated fatty acids may cause several life-threatening diseases, including obesity, diabetes-type 2, cardiovascular diseases, as well as several types of cancer. In this context, a great number of health organizations and government agencies have launched campaigns to reduce the saturated fat content in foods, which has prompted the food industry, which is no stranger to this problem, to start working to develop foods with a lower fat content or with a different fatty acid profile. Nevertheless, this is not an easy task due to the fact that saturated fat plays a very important role in food processing and in the sensorial perception of foods. Actually, the best way to replace saturated fat is with the use of structured vegetable or marine oils. The main strategies for structuring oils include pre-emulsification, microencapsulation, the development of gelled emulsions, and the development of oleogels. This review will examine the current literature on the different (i) healthier oils and (ii) strategies that will be potentially used by the food industry to reduce or replace the fat content in several food products.
... Furthermore, the production of such seed oil turns out to be in line with the uprising trend of the oil industry of seeking for processes that can minimize the environmental impact, decrease toxic residues, and use by-products more efficiently without compromising the nutritional and organoleptic quality of the final product (Cicero et al., 2018; Albergamo et al., 2020). According to the literature, this edible oil exhibits up to 80% of polyunsaturated fatty acids (PUFA), mainly including the ω-6 linoleic acid and the ω-3 α-linolenic acid (Siudem et al., 2019), as well as the γ-linolenic acid, which is typical only of certain seed oils, and the stearidonic acid, which occurs only in few plant families (Matthäus et al., 2008), and whose dietary intake is beneficial to the consumer health, as it promotes the synthesis of the eicosapentaenoic acid more effectively than αlinolenic acid (Lemke 2013). Minor bioactive compounds retained during the cold pressing (e.g., fat-soluble vitamins, phytosterols, polyphenols, pigments, inorganic elements, etc.) have been also highlighted. ...
The cold-pressed hempseed oil (HO) has been increasingly exploited in human diet for its excellent nutritional and healthy properties. However, it has a high content of polyunsaturated fatty acids (PUFAs) and chlorophylls, which inevitably accelerate its oxidative deterioration, especially in presence of light. In this scenario, the filtration technology may ameliorate the oxidative stability of the oil, with positive effects on its nutritional quality and shelf-life. Therefore, in this study, the oxidative stability and minor compounds of non-filtered and filtered HO (NF-HO and F-HO) were monitored over 12 weeks of storage in transparent glass bottles. F-HO showed a better hydrolytic and oxidative status than NF-HO during storage. As a result, F-HO displayed also a better preservation of total MUFA and PUFA in the autoxidation process. Filtration consistently reduced chlorophylls, thus, causing a variation of the natural color of HO. Accordingly, F-HO not only revealed an increased resistance to photooxidation but was also suitable for storage in clear bottles within 12 weeks. F-HO predictably showed lower carotenoids, tocopherols, polyphenols, and squalene compared to NF-HO. However, filtration appeared to play a “protective role” toward these antioxidants, which had lower degradation rates in F-HO than NF-HO for 12 weeks. Interestingly, the element profile of HO was not affected by filtration and remained stable during the study period. Overall, this study may be of practical use to both producers and marketers of cold-pressed HO.
... According to Commission Regulation (EU) 2022/1393 [5], cold-pressed hemp seed oil (CP-HSO) is considered as food derived from hemp seeds, which are the seeds from the industrial type of Cannabis sativa L. The Reg. EU 2022/1393 established the maximum level of delta-9-tetrahydrocannabinol (∆ 9 -THC) equivalents for CP-HSO, i.e., 7.5 mg/kg. CP-HSO is a rich source of polyunsaturated fatty acids (PUFAs) [6] with a ω6:ω3 ratio of around 2.5-3:1, and it is considered optimal from a nutritional point of view and recommended for healthy diets [7,8]. CP-HSO also contains several minor bioactive compounds, such as tocopherols, which are powerful antioxidants and contribute to the prevention of cardiovascular disease [9]. ...
Cold-pressed hemp seed oil (CP-HSO) has become available on the market and is gaining popularity mainly for its appeal and nutritional profile. The sensory quality largely depends on seed quality and processing as well as oil storage conditions. Given the “native” nature of the product, obtained by cold-pressing, the development of a standardized methodology to evaluate and describe the sensory quality of HSOs is of the utmost importance. To this aim, 16 commercial HSOs were evaluated, covering the main differences in brands and sales channels. A trained panel developed a vocabulary to describe the HSO profile consisting of 44 attributes, and a practical sensory wheel was proposed to classify attributes in different clusters and according to sensory modality. A sensory profile sheet was developed including two color descriptors (yellow, green), seven main positive (sunflower/pumpkin seeds, nutty, toasted nutty, hay, sweet, bitter, and pungent), several secondary positive (herbs, coffee, tobacco, etc.), four main defects (rancid, paint, burnt, and fish), and other secondary negative descriptors (boiled vegetables, cucumber, etc.). Subsequently, specific training of the panelists was carried out, and a satisfactory performance level was reached. This study represents the first attempt to standardize the sensory quality and terminology of HSO.
... The total degree of unsaturation was 88.73-89.15% for the Henola cultivar, which is similar to the authors' experiments on other Polish hemp seed oils from the local market [35]. An abundance of essential fatty acids (EFA) was detected for the oils obtained from the Henola cultivar as 72-74% for all varieties, and this was similar to the results obtained for oils extracted by Soxhlet extraction (74-77%) [36]. ...
Cold-pressed hemp (Cannabis Sativa L.) seed oil has become very popular amongst consumers and researchers, due to its manifold application in food and medicine industry. In this study, oils pressed from stored and fresh hemp seeds of the Henola cultivar were analyzed. Determination of the acid value (AV) and color of oil (a* parameter) revealed significant differences between the two groups of oils (fresh and stored seeds) in contrast to the peroxide value (PV), p-anisidine value (p-AV), and fatty acid composition. On the other hand, isothermal and non-isothermal assessments of the thermo-oxidative stability by differential scanning calorimetry (DSC) showed no significant differences in oxidation induction time (OIT) as well as in onset temperature (Ton) between two groups of oils (p > 0.05). The DSC isothermal test (OIT 160) showed significant correlations with mono- and polyunsaturated fatty acids as well as with values of AV and a* (p ≤ 0.05), in contrast to the non-isothermal test, for which correlations were not significant (p > 0.05). However, the best distinction of both groups of oils was obtained analyzing all results together (DSC, fatty acid and tocochromanols composition, color, and oxidative stability results) by principal component analysis (PCA).
... The band at 575 arises from the P-O bonds of PO 4 tetrahedra[61]. The absorption band at 722 cm -1 corresponds to the overlapping of the CH 2 rocking vibrations and out-of-plane CH vibrations[62], suggesting the presence of inadequately decomposed carbon in the LMFP-1 sample. According toFig. ...
Recently, cathode materials for Li-ion batteries (LIBs) with high voltage platforms have become a research hotspot. Olivine-structured LiMnPO4 has the advantage of 4.1 V voltage platform but also has been plagued by poor e⁻/Li⁺ conductivity. Here we report a facile synthetic strategy to fabricate LiMn0.6Fe0.4PO4/C (LMFP) composite. Such composite is composed of [001]-oriented nanorods and assembled into dense microspheres. The [001]-oriented nanorod structure exhibits a shortened Li⁺ diffusion length resulting from a smaller dimensional size in the [010] direction. Meanwhile, the conductive carbon nanolayer is uniformly coated on the surface of LiMn0.6Fe0.4PO4 nanorods, which greatly improves the e⁻ conductivity of the material. The [001]-oriented structure feature combined with improved e⁻ conductivity contribute to the delivery of extraordinary rate capabilities (141.6 mAh g⁻¹ at 10C) and remarkable cycling stabilities (97.8% retention rate after 300 cycles at 1C). Such rational designed nanorod-microspheres are good candidates for the next generation of olivine-structured cathode for high-rate, high-energy, and high-safety LIBs.
... At present, development of additives in animal nutrition attracted wide attention to fulfill the adequate nutrients [3], such as dietary supplement organically chelated copper [4], microencapsulated phytogenic [5], oil [2] and krill meal [6] for dogs. Among them, hemp oil is considered as a beneficial fatty acid resource due to its high content of polyunsaturated fatty acid (80%) [7]. Specifically, a 3:1 ratio of ω-6 linoleic to ω-3 alpha-linolenic acid was recommended for a healthy diet, which is better than other vegetable oils such as olive, soybean, rapeseed and peanut oil. ...
Present study aimed to evaluate the influence of distinct concentration of dietary supplements hemp oil on apparent nutrient digestibility, blood biochemical parameters and metabolomics of teddy dogs. A total of 25 healthy teddy dogs were selected and divided into five treatments according to diet supplements hemp oil at a rate of 0% (A), 0.5% (B), 1% (C), 2% (D), and 4% (E). Appropriate added hemp oil improved apparent nutrient digestibility of dry matter, crude protein and crude fat (86.32-88.08%, 86.87-88.87% and 96.76-97.43%). The hemp oil significantly increased blood biochemical of utilization related total protein, albumin and globulin (61.33-69.54, 35.08-40.38 and 26.53-31.63 g/L), immunity capacity related immunoglobulin E and γ-interferon (203-347kU/L and 23.04-25.78ng/L), energy-related thyroxine and triiodothyronine (27.11-36.75 and 0.94-1.67 nmol/L). In addition, hemp oil improved superoxide dismutation (26.47-33.02 U/ml) and reduced malondialdehyde (5.30-3.28 nmol/ml). The differential metabolites mainly included nucleotides and metabolites of oxidized lipids, bile and other fatty acids, coenzymes and vitamins. The main metabolic pathways included purine and arachidonic acid metabolism, bile and unsaturated fatty acid biosynthesis, cell oxidative phosphorylation and rheumatoid arthritis. Overall, appropriate dietary supplements hemp oil positively to nutrient digestibility and blood metabolism, immunity and antioxidant capacity, 1% to 2% hemp oil supplements was recommended for teddy dog diet.
... The band at 1156 cm − 1 is caused by the bending vibrations of C -O -C, whereas the bands at 1052 and 1028 cm − 1 correspond to C -O stretching vibrations and ring modes. The band at 730 cm − 1 comes from overlapping CH 2 rocking vibrations and out-of-plane C-H vibrations (Geskovski et al., 2021;Siudem et al., 2019). ...
This work describes the application of the liquisolid technique to enhance cannabinoid dissolution from Cannabis sativa L. (CS) compacts. The effects of five vehicles, namely, volatile (ethanol) and nonvolatile (caprylocaproyl macrogolglycerides, polyethylene glycol 400, oleoyl macrogolglycerides and polysorbate 20) liquids, on tablet properties, dissolution and stability were investigated. The viscid oleoresin CS extract was mixed with vehicles before being transformed into free-flowing powder by the use of microcrystalline cellulose and silica as carrier and coating materials. Liquid vehicles had a nonsignificant effect on liquid load factor of CS extract. CS liquisolid compacts had acceptable tableting properties in terms of weight variation, friability, hardness, content uniformity and disintegration time. Different vehicles affected the hardness, disintegration, and wettability of CS compacts and thus the dissolution behaviors of cannabinoids to different extents. Dissolutions of cannabinoids from CS compacts were rate-limited by the disintegration process. Liquisolid formulations using nonvolatile liquids with low polarity or high HLB yielded more than 90% cannabinoid dissolution. Stability studies revealed nonsignificant changes in tablet characteristics, cannabinoid content and dissolutions of CS compacts when stored at 5±3 °C for 3 months. This work presents a general concept of how to successfully formulate CS extract with cannabinoid dissolution enhancement characteristics.
... Health benefits of hemp seed are related to the high level of polyunsaturated fatty acids (PUFAs) present in the seed (Mölleken and Theimer 1997;Kolodziejczyk et al. 2012). Hemp-seed oil does not exert psychotic effect; whereas, it exhibits health beneficial activity due to its optimum proportion of ω-6 linoleic acid and ω-3 alphalinolenic acid (3:1) as recommended in healthy diet (Siudem et al. 2019;Da Porto et al. 2015). Vitamins D and E (fatsoluble vitamins) are other important constituents in hempseed oil. ...
Rising human population has increased the utilization of available resources for food, clothes, medicine, and living space, thus menacing natural environment and mounting the gap between available resources, and the skills to meet human desires is necessary. Humans are satisfying their desires by depleting available natural resources. Therefore, multifunctional plants can contribute towards the livelihoods of people, to execute their life requirements without degrading natural resources. Thus, research on multipurpose industrial crops should be of high interest among scientists. Hemp, or industrial hemp, is gaining research interest because of its fastest growth and utilization in commercial products including textile, paper, medicine, food, animal feed, paint, biofuel, biodegradable plastic, and construction material. High biomass production and ability to grow under versatile conditions make hemp, a good candidate species for remediation of polluted soils also. Present review highlights the morphology, adaptability, nutritional constituents, textile use, and medicinal significance of industrial hemp. Moreover, its usage in environmental conservation, building material, and biofuel production has also been discussed.
... Next, this particular oil is characterized by an optimum ω-6/ω-3 ratio (3:1). Such a property makes it a wholesome oil of a very high nutritive value [22,23]. ...
This paper discusses our attempt to generate substitutes for human breast milk fat through the interesterification of mixtures composed of lard and hemp (Cannabis sativa) seed oil. The interesterification was run at 60 °C for 2, 4, and 6 h in the presence of Lipozyme RM IM preparation containing a lipase specific for the cleavage of sn-1,3 ester bonds in triacylglycerol molecules. The interesterification products were analyzed regarding their fatty acid composition and distribution in triacylglycerol molecules. In order to assess the quality of the generated substitutes, in the interesterification products the following were determined: acid value, peroxide number, and oxidative stability. The collected data were statistically processed using Tukey’s test. Following the interesterification, the fats revealed an elevated percentage of free fatty acids and primary oxidation products and reduced oxidative stability compared to those of lard. The last of the above-mentioned phenomena could have been due to the incorporation of polyenic fatty acids into the external positions of triacyclglycerols of lard. The interesterification of lard and hemp seed oil allows scientists to acquire substitutes rich in essential fatty acids and similar to human breast milk fat with respect to the distribution of fatty acids in triacylglycerol molecules.
... Hempseed oil is a valuable cold-pressed oil with excellent nutritional value. It contains approximately 80% of PUFA, mainly of x-6 linoleic acid and x-3 alpha-linolenic acid (Siudem, Wawer, and Paradowska 2019). Considering the high health benefits, high price, and significant world production of hempseed oil, it is important to establish a fast and efficient detection and quantification method to detect adulteration in this valuable oil. ...
Authenticity and adulteration detection are primary concerns of various stakeholders, such as researchers, consumers, manufacturers, traders, and regulatory agencies. Traditional approaches for authenticity and adulteration detection in edible oils are time-consuming, complicated, laborious, and expensive; they require technical skills when interpreting the data. Over the last several years, much effort has been spent in academia and industry on developing vibrational spectroscopic techniques for quality, authenticity, and adulteration detection in edible oils. Among them, Fourier transforms infrared (FT-IR) spectroscopy has gained enormous attention as a green analytical technique for the rapid monitoring quality of edible oils at all stages of production and for detecting and quantifying adulteration and authenticity in edible oils. The technique has several benefits such as rapid, precise, inexpensive, and multi-analytical; hence, several parameters can be predicted simultaneously from the same spectrum. Associated with chemometrics, the technique has been successfully implemented for the rapid detection of adulteration and authenticity in edible oils. After presenting the fundamentals, the latest research outcomes in the last 10 years on quality, authenticity, and adulteration detection in edible oils using FT-IR spectroscopy will be highlighted and described in this review. Additionally, opportunities, challenges, and future trends of FT-IR spectroscopy will also be discussed.
... Previous investigations from our laboratory reported similar proportions of monounsaturated LA in HSO, but in lower quantities 13 . In our present study, we also detected small quantities of stearidonic and eicosenoic acids, also reported by others 14 (2) Entrapment efficiency(%) = 1 − Determined LA Total LA × 100 21 . LA (ω-6)/ α-linolenic acid (ω-3), and LA (ω-6)/oleic acid (ω-9) ratios were 3.0 and 2.16, respectively. ...
Emerging formulation technologies aimed to produce nanoemulsions with improved characteristics, such as stability are attractive endeavors; however, comparisons between competing technologies are lacking. In this study, two formulation techniques that employed ultrasound and microfluidic approaches, respectively, were examined for relative capacity to produce serviceable oil in water nanoemulsions, based on hempseed oil (HSO). The ultrasound method reached > 99.5% entrapment efficiency with nanoemulsions that had an average droplet size (Z-Ave) < 180 nm and polydispersity index (PDI) of 0.15 ± 0.04. Surfactant concentration (% w/v) was found to be a significant factor (p < 0.05) controlling the Z-Ave, PDI and zeta potential of these nanoparticles. On the other hand, the microfluidic approach produced smaller particles compared to ultrasonication, with good stability observed during storage at room temperature. The Z-Ave of < 62.0 nm was achieved for microfluidic nanoemulsions by adjusting the aqueous : organic flow rate ratio and total flow rate at 4:1 and 12 mL/min, respectively. Further analyses including a morphology examination, a simulated gastrointestinal release behavior study, transepithelial transport evaluations and a toxicity test, using a Caco2-cell model, were performed to assess the functionality of the prepared formulations. The results of this study conclude that both approaches of ultrasound and microfluidics have the capability to prepare an HSO-nanoemulsion formulation, with acceptable characteristics and stability for oral delivery applications.
... The bands in the region 1160-1100 cm −1 are due to stretching vibrations of C-O ester groups (antisymmetric axial stretching and asymmetric axial stretching). The FTIR bands for the CBD oils matched the literature data [41]. The mentioned bands indicate the presence of CBD oil on the surface of the functionalized cotton tampons; regardless of which side was measured, the bands' intensity from the outer side (spectrum B) and from the inner side (spectrum C) are almost identical. ...
The microencapsulation of the cannabidiol and its integration into the tampon can eliminate vaginal inflammation, which at the same time lead to relaxation of the abdominal muscles. The tampon, which contains the active substance cannabidiol (CBD), was developed as an advanced fibrous composite for sanitary application. The active substances were microencapsulated, and, as a carrier, liposomes micro/nano capsules were used. The CBD liposome formulation was analyzed by particle size, polydispersity index, zeta potential, and encapsulation efficiency. Particle size of the CBD liposome liquid formulation was increased by 19%, compared to the liposome liquid formulation and the encapsulation efficiency of CBD in liposome particles, which was 90%. The CBD liposome formulation was applied to cellulose material. The composition of the fibrous composite material was evaluated by Fourier transform infrared spectroscopy, the fiber morphology was analyzed by scanning electron spectroscopy, while the bioactive properties were assessed by antioxidant efficiency, antimicrobial properties, and desorption kinetics. CBD liposome functionalized tampons have both antioxidant and antimicrobial properties. Antimicrobial properties were more pronounced against Gram-positive bacteria. The desorption kinetics of the CBD liposome immobilized on the surface of the composite material was studied using antioxidant activity in the desorption bath. The prepared CBD liposome functionalized tampon additionally shows higher biodegradability compared to references. This high-quality, biodegradable sanitary material based on microencapsulated CBD components as a functional coating provides a platform for many different applications besides medical textiles, also for packaging, pharmaceuticals, paper and wood-based materials, etc.
... The studies [15][16][17][18][19][20] research the fatty acid composition of various hemp oil samples and the ratio of essential polyunsaturated fatty acids ω-6 to ω-3. The generalized fatty acid composition depends on hemp's growing conditions [15] and the extraction of oil from seeds and its refining [16]. ...
Introduction. The work's aim is theoretical and experimental studies of the aspects of industrial hemp seeds' storage technology, as well as the composition and quality of their processed products.
Materials and methods. Research materials are the seeds of industrial hemp of the Hliana variety, press oil, and hemp kernel. To study industrial hemp seeds' composition and quality during long-term storage (12 months), we prepared 12 polypropylene containers filled with the original hemp seeds after their initial processing.
Results and discussion. It was found that the moisture content in the seeds was 8.2–10.0%; seed purity was 97.5– 99.8%; oil content was 31.9–34.3%; the weight of 1000 seeds was 17.7–19.2 g; bulk density of sources was 503,8–530 g/l.
The reduction of the seeds' oil content in the second half of the shelf life was found. The yield of pressurized filtered oil increased at the end of the shelf life. The increase of the oil acid value during the seeds' entire shelf life (0.91–1.46 mg KOH/g) was detected. The peroxide value in the first half of the shelf life of hemp seeds did not exceed 5 ½ O mmol/kg, and in the second half, it increased to 10 ½ O mmol/kg. The primary unsaturated fatty acids in the studied hemp oil are oleic (14.9–19.4%), linoleic (53.4–56.6%), α-linolenic (11.3– 16.2%). The ratio of essential acids ω-6 and ω-3 in the studied oil samples is close to ideal – 3.4:1–5.0:1. The yield of press cake was 67.1–70.0% at the humidity of 6.6–9.0% and at the oil content of 9.5–12.3%. The filter sludge result was 4.6– 8.6% at 4.4–16.8% moisture and 49.2–64.4% oil content. The hemp kernel yield was 33.2–41.4%; content in hemp kernel: moisture – 6.9–7.8%, impurities – 0.01–0.04%. It was established that the oil content in the hemp kernel obtained from the seeds of the Ukrainian selection of the Hliana variety increased by 5.9–8.5% in comparison with the control.
Conclusions. The expediency of using the industrial hemp seeds of the Hliana variety for analytical processing at standardization of storage conditions within a year is proved.
... It achieves a high speed of examination, which needs few to no planning of samples. FTIR spectroscopy has been commonly used as an analytical method in numerous laboratories and sectors, such as foodstuffs [20][21][22], pharmaceuticals [23,24], and control of quality [25,26]. ...
p>Bee pollen is prepared themselves by pollens collecting from plants and has nutritive and therapeutic properties that make it attractive for human health. It has a typical composition related to the botanical origin and geographical location. This study aims to distinguish and identify bee pollen belonging to different Algerian regions and different plants. A methodology for the identification of pollen was developed based on Attenuated Total Reflectance Fourier transform infrared (ATR-FTIR) spectroscopy. This method is simple and fast where samples are not destroyed, also unsupervised statistical methods principal component analysis (PCA) and hierarchical clustering analysis (HCA) are performed. Seventy-two pollen samples were collected and the ATR-FTIR spectra were recorded without processing the samples. ATR-FTIR spectra analysis allowed a reliable determination of the components present in the different samples. Further, PCA and HCA were utilized to evaluate the differences and similarities between the collected samples. Indeed, the PCA score plot and HCA based on ATR-FTIR revealed the same discriminatory trend, where the samples were divided into three main classes based on their total bee pollen. As a result, the PCA along with the HCA was a good and consistent model for identifying and distinguishing pollen grains.</p
... These results are comparable with the ones reported by Prescha et al. (2014) who analysed 12 kinds of cold pressed oils and only in the hempseed oil and rose hip oil found the ω-6 PUFA, GLA, in a percent of 2.2% and 0.1%, respectively. Also, Siudem et al. (2019) when studying the fatty acid composition of six samples of cold pressed hempseed oil found a GLA content ranging between 0.46% and 4.51%, while Teh and Birch (2013) found for the cold pressed hemp oil analysed a content of 4.76% GLA. The cold pressed hempseed oil had a content of SFA, MUFA and PUFA of 8.90%, 16.27% and 74.83%, respectively, comparable with the one reported by Symoniuk et al. (2018) who found the percent of 10.90%, 14.41% and 73.69%, respectively. ...
The objective of this study was to evaluate the nutritional potential of some unrefined vegetable oils in terms of fatty acid composition which was determined by gas chromatography coupled with mass spectrometry. Eight types of vegetable oils, obtained by cold pressing of raw plant materials of sunflower, rapeseed, soybean, flaxseed, sesame, pumpkin, hempseed and walnut were used in the experiments. For all samples, the fatty acid composition was determined individually or as sum of saturated (SFA), monounsaturated (MUFA) and polyunsaturated (PUFA) fatty acids, and omega-6 (ω-6) and omega-3 (ω-3) were also evaluated. Compared with the other tested oils, walnut oil was characterized by the lowest concentrations in SFA (5.33%) and MUFA (15.97%) and the highest concentrations in PUFA (78.70%). Soybean oil had the highest content in SFA (18.70%), while the rapeseed oil was characterized by the highest content in MUFA (67.49%) and the lowest content in PUFA (24.74%). Nutritional claims regarding the MUFA content can be made for rapeseed oil, while for the other tested oils can be mentioned that are high in PUFA. The soybean, rapeseed, flaxseed, hempseed and walnut cold pressed oils can be considered to have nutritional potential due to the high amounts of ω-3 PUFA.
... Oil extracted through hemp seed is rich in ω-6 linoleic and ω-3 α-linolenic fatty acids. It is rare and unique plant to possess the ratio of ω-6/ω-3 in 3:1, which is known to be the most suitable ratio for vegetarian diet [2][3][4][5]. It improves the oil quality, which is beneficial for various health problems such as flammation [5], bad immunity [2], etc. ...
In the present work, supercritical fluid extraction (SFE) of hemp ( Cannabis sativa ) seed oil at various ranges of SFE parameters is performed. These parameters and respective ranges are temperature (40–80) °C, pressure (200–350) bar, solvent (CO 2 ) flow rate (5–15) g/min, particle size (0.43–1.02) mm and amount of co-solvent (ethanol) (0–10) % of solvent flow rate. Central composite design (CCD) suggests 32 experimental runs to perform through SFE. The obtained oil is analysed through gas chromatography to identify its fatty acids concentrations. The ratio of ω-6 linoleic and ω-3 α-linolenic fatty acids (ω-6/ω-3) is optimized through CCD to obtain the desired amount of 3:1 as this ratio is highly preferred for various health benefits. Ratio of ω-6/ω-3 is obtained in the range from 2.11 to 3.06:1 for all experimental runs. The effect of SFE parameters on this ratio is investigated. Further, cross-validation is peformed on the experimental data obtained for the concentrations of both fatty acids by jackknife and bootstrap resampling to authenticate the obtained data. Small value of standard deviation (~1), less standard error of the mean (SEM) (<0.8) and less variance coefficient (<0.11) confirms the validity of the obtained data. All the estimators’ values such as standard deviation, variance coefficients and SEM are observed in 95 % of confidence intervals.
In vivo plant hormonal detection methods are the strategies executed on living organisms while not taking out the samples from the body. Modern methods like spectroscopy, biosensors, and electrochemical sensors have increased the quality and sensitivity of the detection and decreased the cumbersome, time, and solvent-consuming preparational efforts of traditional methods. Preparational efforts generally consisted of several samplings, extraction, purification, and enrichment steps to analyze plant hormones. Concentrations and levels of plant hormones change concerning biotic and abiotic stresses that plant faces. Spectroscopy, biosensors, and electrochemical sensors detect different plant hormones with specific accuracy and desired results, but their handling and sample preparations are challenging. At the same time, advanced ultrasensitive nondestructive methods are biocompatible and can be used for a lifetime with excellent stretchability performance. In modern science, portable, wearable, and nondestructive measurement is the trend of plant sensors that can make the “Internet of Plants” concept a reality. This review covers the significant aspects of numerous applications, advantages, and disadvantages of spectroscopy, biosensors, electrochemical sensors, and new ultrasensitive nondestructive devices to measure in vivo plant hormones. The summary of the advanced ultrasensitive plant devices, their challenges, and future prospects within the fields for in vivo plant hormone detections is presented. Furthermore, it can guide researchers to design new experiments using ultrasensitive nondestructive sensing devices for detecting in vivo plant hormones.
Cold-pressed hempseed oil (HO) has been increasingly exploited in the human diet for its excellent nutritional and healthy properties. However, it has a high content of polyunsaturated fatty acids (PUFAs) and chlorophylls, which inevitably accelerate its oxidative deterioration, especially in the presence of light. In this scenario, the filtration technology may ameliorate the oxidative stability of the oil, with positive effects on its nutritional quality and shelf life. Therefore, in this study, the oxidative stability and minor compounds of non-filtered and filtered HO (NF-HO and F-HO) were monitored over 12 weeks of storage in transparent glass bottles. F-HO showed a better hydrolytic and oxidative status than NF-HO during storage. As a result, F-HO also displayed better preservation of total MUFAs and PUFAs in the autoxidation process. Filtration consistently reduced chlorophylls, thus causing a variation in the natural color of HO. Accordingly, F-HO not only revealed an increased resistance to photooxidation but it was also suitable for storage in clear bottles within 12 weeks. F-HO predictably showed lower carotenoids, tocopherols, polyphenols, and squalene compared to NF-HO. However, filtration appeared to play a "protective role" toward these antioxidants, which had lower degradation rates in F-HO than NF-HO for 12 weeks. Interestingly, the element profile of HO was not affected by filtration and remained stable during the study period. Overall, this study may be of practical use to both producers and marketers of cold-pressed HO.
The decarboxylation of Δ9-tetrahydrocannabinolic acid (THCA) plays pivotal role in the potency of medical cannabis and its extracts. However, the literature data point out substantial variations in the process reaction rate and conversion efficacy due to variability of the temperature, heat transfer efficacy, raw material attributes, consequently resulting in incomplete decarboxylation, cannabinoid content decrease due to decomposition, evaporation, and possible side reactions. Our present work aims to draw attention to mid-infrared (MIR) spectroscopy for in-situ monitoring and decipher the THCA decarboxylation reaction in the solid state. The initial TG/DTG curves of THCA, for a first time outlined the solid-solid decarboxylation dynamics, defined the endpoint of the process and the temperature of the maximal conversion rate, which aided in the design of the further IR experiments. Temperature controlled IR spectroscopy experiments were performed on both THCA standard and cannabis flower by providing detailed band assignment and conducting spectra-structure correlations, based on the concept of functional groups vibrations. Moreover, a multivariate statistical analysis was employed to depict the spectral regions of utmost importance for the THCA→THC interconversion process. The principal component analysis model was reduced to two PCs, where PC1 explained 94.76% and 98.21% of the total spectral variations in the THCA standard and in the plant sample, respectively. The PC1 plot score of the THCA standard, as a function of the temperature, neatly complemented to the TG/DTG curve and enabled determination of rate constants for the decarboxylation reaction undertaken on several temperatures. Consequently, a progress in elucidation of kinetic models of THCA decarboxylation, fitting experimental data for both, solid state standard substance and a plant flower, was achieved. The results open the horizon to promote an appropriate process analytical technology (PAT) in the outgrowing medical cannabis industry.
Введение: Повышение пищевой ценности рационов питания населения относится к приоритетным задачам национального и международного уровня. Мучные кондитерские изделия представляют собой перспективную основу для обогащения их функциональными ингредиентами. Семена конопли и продукты их переработки вызывают научный интерес в исследованиях области питания. В последние годы обсуждение данного сырья заметно возросло ввиду создания сортов технической конопли с низким содержанием наркотических компонентов – тетрагидроканнабинола (ТГК) (0,1…0,3%), легализации возделывания и ее переработки. В связи с этим использование продуктов переработки семян конопли является актуальным направлением, однако, недостаточно изученным.Цель: Изучение эффективности использования продуктов переработки семян конопли для повышения пищевой ценности мучных кондитерских изделий. Материалы и методы: В данном исследовании изучались продукты переработки семян конопли – конопляная мука, измельченное ядро семян конопли, обрушенные семена конопли, белковый концентрат из семян конопли, измельченные семена конопли, конопляное масло и клетчатка семян конопли, в качестве добавок при изготовлении мучных кондитерских изделий. Исследуемые образцы вносились при замесе теста в рецептуру маффинов.Результаты: Физико-химические показатели определялись стандартными методами анализа. Плотность образцов по сравнению с контролем менялась в зависимости от вносимой добавки. При внесении клетчатки и конопляного масла плотность образцов увеличивалась (0,58 и 0,56 г/см3 соответственно). Добавление измельченных семян конопли и муки из семян конопли напротив приводили к снижению плотности образцов – 0,41 г/см3 каждый. Обрушенные семена конопли, белковый концентрат и клетчатка семян конопли положительно влияли на упек образцов (15,87, 16,15 и 16,26% соответственно). Отмечено, что лучший удельный объем был у образца с содержанием 10% конопляной муки – 2,54 см3/г. В результате хранения все продукты переработки семян конопли снижали скорость черствения маффинов. Установлено, что лучшими органолептическими показателями обладали маффины с конопляным маслом, которое полностью заменяло подсолнечное масло в рецептуре образцов. Также высокой комплексной оценкой по органолептическим показателям обладали образцы с конопляной клетчаткой (5%). По уровню энергетической ценности полученные образцы относят к продуктам со средней энергетической ценностью.Выводы: Расширение ассортимента пищевых продуктов, содержащих добавки семян конопли и продуктов их переработки, а также активное потребление населением этих изделий будет содействовать реализации национальных программ по оздоровлению населения.
Purpose
Hempseed oil is a valuable emerging food product with recognized health positivity due to its composition. The paper aims to propose a multi-methodological chemical profiling of nine organic hempseed oil samples (different brands and prices) from the retail market, followed by multivariate data analysis.
Design/methodology/approach
Fatty acids, tocopherols, squalene, total carotenoids content, phenolic compounds, total phenolic content and anti-radical activity (DPPH• and ABTS•+ assays) were determined through chromatographic and spectrophotometric techniques. Multivariate (explorative and discriminant) analyses were applied to the profiling results to classify samples according to information claimed on the label, i.e. geographical origin (EU vs. non-EU), extraction procedure (cold-pressed vs. not cold-pressed) and price (lower or higher than 10 € per 250 mL).
Findings
The chemical analysis confirmed the 3 to 1 ?-6:?-3 ratio and the excellent content in antioxidant species. However, no specific trend of results can be stressed. PCA (after variables selection) highlighted a natural grouping of samples, so three discriminant analyses were performed: kNN, Naïve Bayes and LDA. The best classification efficiency was reached for the extraction procedure verification (93–100% correct classification), followed by geographical origin (83–94%) and prices (81.6–90%).
Originality/value
The integrated approach of chemical profiling coupled with multivariate analyses allowed the assessment of label information of the analyzed organic hempseed oil samples, despite the wide heterogeneity of the selected samples.
The fatty acid composition is a parameter that determines the quality and origin of vegetable oils. The standard method used in the analysis of fatty acid composition is gas chromatography (GC). In the last 20 years, however, the ¹H NMR method has become more important in the analysis of fatty acids. Thanks to no need of special sample preparation, the high speed of analysis and the possibility to automate the process of analysis, ¹H NMR is becoming a popular method of testing vegetable oils. It is possible to test oils both qualitatively and quantitatively, taking into account both the fatty acid profile and the level of minor components. In combination with statistical and chemometric methods, the analysis of ¹H NMR spectra allows one to obtain much valuable information about the tested oil, considering its composition, quality, the presence of impurities, or the origin. The paper presents an overview of publications focusing on the application of the ¹H NMR method in the profiling of fatty acids in vegetable oils.
Hemp oil is widely used in the food industry, and also in many other industries. It is characterized by a high content of unsaturated fatty acids with the optimal ratio of ω-6 to ω-3 fatty acids (3:1). Such composition means that this oil is often used in the food, pharmaceutical and cosmetic industries. Due to the popularity of hemp oil and its high content of unsaturated fatty acids, methods for the quick oil quality analysis are sought. Six samples of cold-pressed hemp oil were stored under different conditions (2-8°C and 30°C) for one month and then their ¹H NMR spectra were recorded. The chemometric methods of PCA and OPLS-DA were used to perform the analysis of the spectra. The combination of those methods made it possible to observe the differences in the oil samples after a month of storage. Based on the ¹H NMR spectra, it was possible to differentiate the time and conditions of the oil storage.
Industrial hemp hearts were subjected to three different extraction techniques-advanced extraction techniques like microwave and ultrasound extraction and primitive extraction technique like mechanical cold pressing in order to extract oils. The extraction yield varied between 41.0 ± 2.1 % (w/w) and 54.0 ± 2.7 % (w/w). Linoleic acid (LA) was reported to be the major polyunsaturated fatty acid (PUFA) followed by α−Linolenic acid (ALA). The ratio of LA to ALA was found to be close to 3:1 which is considered optimal for nutrition. The ratio of unsaturated fatty acids (UFA) to saturated fatty acids (SFA) was in the range of 6.7 to 9.1. Several minor compounds like ɣ-Sitosterol, stigmasterol, rhodoxanthin, carotene, and methyl cholate as well as antioxidants like β-Carotene and ɣ-Tocopherol have been identified in the oils. The physicochemical properties of the oils like the acid value, iodine value, and oxidative stability indicated that they have higher quality and that the level of unsaturation was very high. Furthermore, free radical scavenging activity of the oils revealed that the oils exhibited 94 % of activity in the first 2 h. A perfect combination of unsaturated fatty acids and saturated fatty acids, an appropriate medley of different antioxidants not only qualifies hemp seed oil as an excellent source of nutrition but also as an important plant-based (vegetable) oil for the higher value nutraceutical and pharmaceutical industries.
Bal arıları meyve, sebze ve tohum oluşumu için çok önemli hayvanlardır.
Arılar, çiçekli bitkilerin erkek yapılarındaki polenleri dişi kısımlarına
aktararak bitkilerde meyve ve tohum oluşumunu sağlar. Ayrıca bal
yapmaları nedeniyle de tarih boyunca bu böceklere çok önem verilmiştir.
Biz insanlar her zaman bal arısına hayran olmuşuzdur. Afrika, Avrupa
ve Asya’daki en eski atalarımız, yüz binlerce yıl boyunca, bu arının bal
depolama ve balmumu yapma konusundaki şaşırtıcı endüstrisine, çok
değerli iki maddeye kesinlikle hayran kaldılar. Daha yakın zamanlarda,
son 10.000 yılda, karmaşık arıcılık zanaatını icat ettik ve bal arıları
üzerine bilimsel çalışmalarımıza başladık. Örneğin, bu arının «çiçek
değişmezliği» uygulamasını ilk kez tanımlayan antik filozof Aristotales’ti:
Bir işçi arı, yiyecek toplamanın verimliliğini artırmak için yiyecek
arama gezisi boyunca genellikle bir tür çiçeğe yapışır. Bal arısının
doğal dünyasında nasıl yaşadığını bilmek, geniş bir bilimsel araştırma
yelpazesi gerekmektedir. Bunun nedeni, Apis mellifera’nın biyolojideki,
özellikle davranışla ilgili temel soruları araştırmak için model sistemlerden
biri haline gelmesidir. Bu arıları ister hayvan bilişindeki, ister
davranışsal genetikteki veya sosyal davranışlardaki bazı gizemleri çözmek
için çalışıyor olun, birinin deneysel araştırmalarını tasarlamadan
önce doğal biyolojilerine aşina olmak kritik derecede önemlidir.
This chapter introduces the principles and practice of various analytical methods important for characterizing herbal biomolecules that include both primary and secondary metabolites. It offers scientists a survey of common analytical techniques including ultraviolet-visible, fluorescence, polarimetry, circular dichroism, fourier transform-infrared spectroscopy, nuclear magneteic resonance, single-crystal X-ray diffraction, mass spectrometry, liquid chromatography, gas chromatography, thin layer chromatography, immunoassays, gel and capillary electrophoresis and DNA and protein sequencing. The discussion of each technique is further illustrated by its application to characterize specific herbal biomolecules, including Amaryllidaceae alkaloids, tropane alkaloids, terpenes, phenolic compounds, glycosides, polysaccharides, DNA, RNA, protein and peptides. The chapter highlights the critical roles of analytical techniques in characterizing the complex structures and determining the composition of the herbal biomolecules to better understand herbal quality and biological action in healthcare and diseases.
O açaizeiro (Euterpe oleracea Mart.) é uma palmeira nativa da Amazônia, que ocorre em grandes extensões no estuário amazônico. Durante o processo de conservação e extração de óleos, fatores como umidade, temperatura, enzimas lipídicas e presença de luz, podem afetar o perfil lipídico, favorecendo a hidrólise e liberando ácidos graxos. A presença de ácidos graxos influencia na qualidade dos óleos. Este trabalho teve como objetivo a extração do óleo de açaí por solvente orgânico e a análise de alguns parâmetros físico-químicos como: densidade, níveis de acidez, e perfil glicídico. Para a extração foram utilizados o aparelho soxhlet e o hexano como solvente. A extração do óleo de açaí não apresentou bom rendimento, devido à escolha de se utilizar os frutos inteiros que tem grandes quantidades de fibras envoltas nas sementes. A densidade foi analisada através do densímetro 35n da ANTON PAAR, a acidez foi medida através de titulação por KOH e para o perfil glicídico o óleo foi submetido a análise de espectroscopia no infravermelho por transformada de Fourier (FTIR), utilizando o aparelho IR Prestige-21 da Shimadzu. A densidade apresentou-se um pouco baixa. O nível de acidez apresentou valores um pouco elevados, indicando a formação de ácidos graxos, no perfil glicerídeo foi possível observar a presença de ácidos graxos livres, o que justifica a acidez.
Industrial hemp (Cannabis sativa L.), as one of the most important traditional natural fiber crops, had almost been forgotten for the last several decades. However, an unprecedented opportunity has emerged for planting this crop due to its multiple uses and products derived from the plant as well as its quick-growing and strong adaptability to a wide range of agro-environmental conditions. Furthermore, the decision from the United Nations’ Commission for Narcotic Drugs that removing medicinal cannabis from a category of dangerous drugs (Schedule IV of the Single Convention on Narcotic Drugs, 1961) in December 2020 has also greatly promoted the hemp’s revival. Nowadays, industrial hemp has many agro-industrial applications, such as agriculture, textiles, papermaking, construction, bio-fuel. This review analyzes the current hemp production status throughout the world and outlines the main applications of industrial hemp in different fields. The outlook and the remaining questions that need to be solved in the future for the better development of industrial hemp were also discussed, such as how to promote the hemp planting in more broad regions, how to obtain high yields of aim products, and how to fully explore its usages in the future.
Infrared (IR) spectral analysis via Fourier transform infrared spectroscopy, second derivative infrared spectroscopy, dual-index sequential analysis and antioxidant activity evaluation was conducted to analyze the differences of Dictamnus dasycarpus Turcz (DdT) in different growth years. The position, intensity and shape of the characteristic peaks on IR spectra all differed among different growth years. With the prolonging of growth time, the amount of DdT accumulating in the metabolism substances gradually increased, characteristic peaks appeared at 3420, 2927, 1739, 1670, 1620, 1511, 1230, 989 and 806 cm⁻¹, and the main chemical components were dictamnine, obacunone and fraxinellone. Antioxidant activity evaluation showed all four samples possessed high scavenging activities against 1,1-Diphenyl-2-picrylhydrazyl radical (DPPH∙) and 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) radical (ABTS+), and the activity was strengthened with the increase of growth years. The two-step IR macro-fingerprint identification and bioactivity analysis indicated the potential extension of this technique for identification and discrimination of DdT. This should be beneficial to providing a technical basis for identification and picking of DdT and other natural products in the future.
The quantification of cannabinoids is an essential part of cannabis profiling and testing, whether for medical or recreational use. As regulatory bodies continue to increase testing requirements for these products, it is crucial that alternative and effective analytical methods be developed. Herein, we describe the use of benchtop NMR instruments for the quantification of Δ⁹-tetrahydrocannabinol (THC) and cannabidiol (CBD) in a variety of cannabis concentrates and compare the values to those obtained using HPLC, the most common approach for the quantification of cannabinoids. Based on the discrepancies observed in test values from different laboratories using only HPLC, the value of orthogonal testing methods has been identified and is increasingly desired.
Adulterated sesame oil seriously damages the interests of consumers and the health of market. In this paper, a simple, fast and real-time model for identifying adulterated sesame oil (ASO) was proposed by combining 3D fluorescence spectra with wavelet moments (WMs). First, noise and data volume of the experimental data were reduced by wavelet multiresolution decomposition (WMRSD), which improved the stability and real-time of the model. Next, WMs were used to extract the features of the 3D fluorescence spectra and proved to be effective by hierarchical clustering results. Then, the qualitative quality of WMs of the same orders, different orders and the combinations were evaluated by Dunn's validity index (DVI), and the rules were given, respectively. Finally, the target WMs for identifying ASO were determined. This model is simple and fast, and expandable to online measurement, providing a reference for identification and adulteration of vegetable oils.
The study describes the curing and thermal behaviour of a new castor oil maleic anhydride adduct/epoxy oils/5–Bromosalicylic acid coatings and their composites with wood. The epoxidized oils were flax and hemp. The kinetic parameters of the curing and thermal degradation processes were calculated. The resistance of the coated wood surfaces against Cladosporium cladosporioides, Aspergillus brasiliensis and Penicillium chrysogenum was tested. Colour changes, FT–IR and SEM were conducted before and after fungal attack. The decay resistance and colour change of raw wood and wood treated samples against fungi was tested. Based on the colour changes and according to ASTM D 2017, the decay resistance rating for covered samples was considered as “highly resistant”. Chemical resistance and coating performance tests were also undertaken. The obtained results recommend the described materials for applications in wood protective coatings.
In this work, we introduce an NMR-based screening method for the fatty acid composition analysis of edible oils. We describe the evaluation and optimization needed for the automated analysis of vegetable oils by low-field NMR to obtain the fatty acid composition (FAC). To achieve this, two scripts, which automatically analyze and interpret the spectral data, were developed. The objective of this work was to drive forward the automated analysis of the FAC by NMR. Due to the fact that this protocol can be carried out at low field and that the complete process from sample preparation to printing the report only takes about 3 min, this approach is promising to become a fundamental technique for high-throughput screening. To demonstrate the applicability of this method, the fatty acid composition of extra virgin olive oils from various Spanish olive varieties (arbequina, cornicabra, hojiblanca, manzanilla, and picual) was determined by ¹H-NMR spectroscopy according to this protocol.
This study was undertaken to evaluate the clinical efficacy, safety, and histological changes induced by dietary omega-3 fatty acid and γ-linoleic acid in acne vulgaris. A 10-week, randomised, controlled parallel dietary intervention study was performed in 45 participants with mild to moderate acne, which were allocated to either an omega-3 fatty acid group (2,000 mg of eicosapentaenoic acid and docosahexaenoic acid), a γ-linoleic acid group (borage oil containing 400 mg γ-linoleic acid), or a control group. After 10 weeks of omega-3 fatty acid or γ-linoleic acid supplementation, inflammatory and non-inflammatory acne lesions decreased significantly. Patient subjective assessment of improvement showed a similar result. Heamatoxylin and eosin staining of acne lesions demonstrated reductions in inflammation and immunohistochemical staining intensity for interleukin-8. No severe adverse effect was reported. This study shows for the first time that omega-3 fatty acid and γ-linoleic acid could be used as adjuvant treatments for acne patients.
Cold-pressed oil content of Cannabis sativa (hemp) seeds from three different agro-ecological zones of Pakistan ranged from 26.90 to 31.50%. Protein, fiber, ash, and
moisture content were found to be 23.00–26.50, 17.00–20.52, 5.00–7.60, and 5.60–8.50%, respectively. Results of some other
physical and chemical parameters of the oil were as follows: iodine value, 154.00–165.00; refractive index (40°C), 1.4698–1.4750;
density (24°C), 0.9180–0.9270 mg ml−1; saponification value, 184.00–190.00; unsaponifiable matter, 0.70–1.25%; and color (1-in cell), 0.50–0.80 R+27.00–32.00 Y.
The induction period (Rancimat, 20 L h−1, 120°C) of the nondegummed and degummed oils ranged from 1.35 to 1.72 h and from 1.20 to 1.49 h, respectively. Specific extinctions
at 232 and 270 nm were 3.50–4.18 and 0.95–1.43, respectively. The hemp oils investigated were found to contain high levels
of linoleic acid, 56.50–60.50%, followed by α-linolenic, oleic, palmitic, stearic, and γ-linolenic acids: 16.85–20.00, 10.17–14.03,
5.75–8.27, 2.19–2.79, and 0.63–1.65%, respectively. Tocopherols (α, γ, and δ) in the nondegummed oils were found to be 54.02–60.40,
600.00–745.00, 35.00–45.60, respectively, and were reduced to 29.90–50.00, 590.00–640.00, and 30.40–39.50 mg kg−1, respectively, after degumming. The results of the present analytical study, compared with those found in the typical literature
on hempseed oils, showed C. sativa indigenous to Pakistan to be a potentially valuable nonconventional oilseed crop of comparable quality.
Several sources of information suggest that human beings evolved on a diet with a ratio of omega-6 to omega-3 essential fatty acids (EFA) of approximately 1 whereas in Western diets the ratio is 15/1-16.7/1. Western diets are deficient in omega-3 fatty acids, and have excessive amounts of omega-6 fatty acids compared with the diet on which human beings evolved and their genetic patterns were established. Excessive amounts of omega-6 polyunsaturated fatty acids (PUFA) and a very high omega-6/omega-3 ratio, as is found in today's Western diets, promote the pathogenesis of many diseases, including cardiovascular disease, cancer, and inflammatory and autoimmune diseases, whereas increased levels of omega-3 PUFA (a lower omega-6/omega-3 ratio), exert suppressive effects. In the secondary prevention of cardiovascular disease, a ratio of 4/1 was associated with a 70% decrease in total mortality. A ratio of 2.5/1 reduced rectal cell proliferation in patients with colorectal cancer, whereas a ratio of 4/1 with the same amount of omega-3 PUFA had no effect. The lower omega-6/omega-3 ratio in women with breast cancer was associated with decreased risk. A ratio of 2-3/1 suppressed inflammation in patients with rheumatoid arthritis, and a ratio of 5/1 had a beneficial effect on patients with asthma, whereas a ratio of 10/1 had adverse consequences. These studies indicate that the optimal ratio may vary with the disease under consideration. This is consistent with the fact that chronic diseases are multigenic and multifactorial. Therefore, it is quite possible that the therapeutic dose of omega-3 fatty acids will depend on the degree of severity of disease resulting from the genetic predisposition. A lower ratio of omega-6/omega-3 fatty acids is more desirable in reducing the risk of many of the chronic diseases of high prevalence in Western societies, as well as in the developing countries.
Lipid metabolism, inflammation, oxidative stress and endothelial function play important roles in the pathogenesis of cardiovascular disease (CVD), which may be affected by an imbalance in the n-6/n-3 polyunsaturated fatty acid (PUFA) ratio. This study aimed to investigate the effects of the n-6/n-3 PUFA ratio on these cardiovascular risk factors in rats fed a high-fat diet using plant oils as the main n-3 PUFA source. The 1:1 and 5:1 ratio groups had significantly decreased serum levels of total cholesterol, low-density lipoprotein cholesterol, and proinflammatory cytokines compared with the 20:1 group (p < 0.05). Additionally, the 20:1 group had significantly increased serum levels of E-Selectin, von Willebrand factor (vWF), and numerous markers of oxidative stress compared with the other groups (p < 0.05). The 1:1 group had a significantly decreased lipid peroxide level compared with the other groups (p < 0.05). Serum levels of malondialdehyde, reactive oxygen species and vWF tended to increase with n-6/n-3 PUFA ratios increasing from 5:1 to 20:1. We demonstrated that low n-6/n-3 PUFA ratio (1:1 and 5:1) had a beneficial effect on cardiovascular risk factors by enhancing favorable lipid profiles, having anti-inflammatory and anti-oxidative stress effects, and improving endothelial function. A high n-6/n-3 PUFA ratio (20:1) had adverse effects. Our results indicated that low n-6/n-3 PUFA ratios exerted beneficial cardiovascular effects, suggesting that plant oils could be used as a source of n-3 fatty acids to prevent CVD. They also suggested that we should be aware of possible adverse effects from excessive n-3 PUFA.
In this study, 44 samples, either pure or combined into binary blends of vegetable oils with different botanical and geographical origin have been analyzed. 1H and 13C NMR analysis was used to determine the saturated fatty acids, oleic acid, linoleic acid, linolenic acid and iodine value. Oil samples were separated according to the botanical origin using principal component analysis. Results found virgin olive oils clustered close together in spite of the different geographical origin while walnut oil varied greatly with country of origin. Blends of 1% olive oil in sun-flower oil were detected using specific 1H and 13C signals. The results strongly support the capability of NMR and chemometrics to be used in quality assessment of vegetable oils in terms of their botanical origin.
http://authors.elsevier.com/a/1PnmQ3PY0v9sW4
ABSTRACT The cultivation of four industrial hemp cultivars (Felina 32, Chamaeleon, Uso31, and Finola) was investigated for oil production in the north-east of Italy along two years. The oils of all cultivars resulted in rich amount of linoleic acid (ω-6) and α-linolenic acid (ω-3). Felina 32 and Chamaeleon oils exhibited the highest amount of linoleic acid (59%) and α-linolenic acid (18%). Finola and Uso31 oils resulted in the richest of γ-linolenic acid (5-6%). All hempseed oils presented high oxidation stability and an acceptable initial quality. It is suggested that these oils can be used to produce EFA dietary supplements high in ω-6 and ω-3 of vegetal origin.
Aldehydes, formed as secondary oxidation products during the autoxidation process of oils and fats, are analytical markers used to assess the lipid deterioration status. Generally, the level of aldehydes is expressed as the p-anisidine value (AV). This deterioration index is based on the reaction of the carbonyl group with p-anisidine leading to the formation of an intensively coloured Schiff base which is determined spectroscopically (UV/ViS). 1H NMR provides an alternative approach by enabling the quantification of individual aldehydes like n-alkanals, 2-alkenals or (E,E)-2,4-alkadienals. This work illustrates that the AV can be modelled as a linear combination of the NMR integrals of aldehydes. A functional relationship was derived on the basis of calibration experiments. The suitability of the model is shown by comparing the NMR-determined AVs with the classical AVs of 79 commercially available edible oils of different oil types.
Supercritical carbon dioxide (SC-CO2) was employed to extract oil from hemp (Cannabis sativa L.) seeds. For ground seeds, the supercritical extraction was carried out at temperatures of 40, 60 and 80 °C and pressures of 300 and 400 bar. Different solvent-ratios were applied. Supercritical CO2 extractions were compared with a conventional technique, n-hexane in Soxhlet. The extraction yields, fatty acid composition of the oil and oxidation stability were determined. The seed samples used in this work contained 81% PUFAs, of which 59.6% was linoleic acid (ω-6), 3.4% γ-linolenic (ω-3), and 18% α-linolenic (ω-6). The highest oil yield from seeds was 22%, corresponding to 72% recovery, at 300 bar and 40 °C and at 400 bar and 80 °C. The highest oxidation stability corresponding to 2.16 mM Eq Vit E was obtained at 300 bar and 80 °C.
Indices like acid value, peroxide value, and saponification value play an important role in quality control and identification of lipids. Requirements on these parameters are given by the monographs of the European pharmacopeia. (1)H NMR spectroscopy provides a fast and simple alternative to these classical approaches. In the present work a new (1)H NMR approach to determine the acid value is described. The method was validated using a statistical approach based on a variance components model. The performance under repeatability and in-house reproducibility conditions was assessed. We applied this (1)H NMR assay to a wide range of different fatty oils. A total of 305 oil and fat samples were examined by both the classical and the NMR method. Except for hard fat, the data obtained by the two methods were in good agreement. The (1)H NMR method was adapted to analyse waxes and oleyloleat. Furthermore, the effect of solvent and in the case of castor oil the effect of the oil matrix on line broadening and chemical shift of the carboxyl group signal are discussed.
Nuclear Magnetic Resonance (NMR) Spectroscopy has been extensively used for the analysis of olive
oil and it has been established as a valuable tool for its quality assessment and authenticity. To date,
a large number of research and review articles have been published with regards to the analysis of
olive oil reflecting the potential of the NMR technique in these studies. In this critical review, we cover
recent results in the field and discuss deficiencies and precautions of the three NMR techniques (1H, 13C,
31P) used for the analysis of olive oil. The two methodological approaches of metabonomics, metabolic
profiling and metabolic fingerprinting, and the statistical methods applied for the classification of olive
oils will be discussed in critical way. Some useful information about sample preparation, the required
instrumentation for an effective analysis, the experimental conditions and data processing for obtaining
high quality spectra will be presented as well. Finally, a constructive criticism will be exercised on the
present methodologies used for the quality control and authentication of olive oil.
Examples of the application of green chemistry in the analytical laboratory are presented. The principles of this approach include primary elimination or at least reduction of the amounts of reagents and solvents during laboratory work, particularly at the sample preparation stage.
Virgin hemp seed oil is not widespread on the market, although it is characterised by an interesting fatty acid composition with a high content of polyunsaturated fatty acids. Linoleic acid is the predominant fatty acid, which comes, together with α-linolenic acid (18:3n-3), to approximately 80% of the total fatty acids. From a nutritional point of view, up to 7% γ-linolenic acid (18:3n-6) and 2.5% stearidonic acid (18:4n-3) are very interesting. The total amount of tocopherols is high between 80 and 110 mg/100 g, with γ-tocopherol as the main tocopherol (85%). Due to the high amount of unsaturated fatty acids, hemp seed oil is very susceptible to oxidative deterioration, which results in a fast impairment of the oil during storage. In addition, the high amounts of chlorophyll in the oil due to harvesting of high amounts of immature seeds require light protection, which is often neglected because of merchandising purposes. The virgin oil is characterised by a nutty taste with a slightly bitter aftertaste. The use of virgin hemp seed oil is recommended during mild processing of food without heat.
Rapid Fourier transform infrared (FTIR) spectroscopy combined with attenuated total reflectance (ATR) was applied for quantitative
analysis of virgin coconut oil (VCO) in binary mixtures with olive oil (OO) and palm oil (PO). The spectral bands correlated
with VCO, OO, PO; blends of VCO and OO; VCO and PO were scanned, interpreted, and identified. Two multivariate calibration
methods, partial least square (PLS) and principal component regression (PCR), were used to construct the calibration models
that correlate between actual and FTIR-predicted values of VCO contents in the mixtures at the FTIR spectral frequencies of
1,120–1,105 and 965–960cm−1. The calibration models obtained were cross validated using the “leave one out” method. PLS at these frequencies showed the
best calibration model, in terms of the highest coefficient of determination (R
2) and the lowest of root mean standard error of calibration (RMSEC) with R
2=0.9992 and RMSEC=0.756, respectively, for VCO in mixture with OO. Meanwhile, the R
2 and RMSEC values obtained for VCO in mixture with PO were 0.9996 and 0.494, respectively. In general, FTIR spectroscopy serves
as a suitable technique for determination of VCO in mixture with the other oils.
KeywordsFTIR-Virgin coconut oil-Binary mixture-Partial least square-Principal component regression
One hundred and thirty-eight oil samples have been analyzed by visible and near-infrared transflectance spectroscopy. These comprised 46 pure extra virgin olive oils and the same oils adulterated with 1% (w/w) and 5% (w/w) sunflower oil. A number of multivariate mathematical approaches were investigated to detect and quantify the sunflower oil adulterant. These included hierarchical cluster analysis, soft independent modeling of class analogy (SIMCA method), and partial least squares regression (PLS). A number of wavelength ranges and data pretreatments were explored. The accuracy of these mathematical models was compared, and the most successful models were identified. Complete classification accuracy was achieved using 1st derivative spectral data in the 400-2498 nm range. Prediction of adulterant content was possible with a standard error equal to 0.8% using 1st derivative data between 1100 and 2498 nm. Spectral features and chemical literature were studied to isolate the structural basis for these models.
A combination of (1)H NMR and (31)P NMR spectroscopy and multivariate statistical analysis was used to classify 192 samples from 13 types of vegetable oils, namely, hazelnut, sunflower, corn, soybean, sesame, walnut, rapeseed, almond, palm, groundnut, safflower, coconut, and virgin olive oils from various regions of Greece. 1,2-Diglycerides, 1,3-diglycerides, the ratio of 1,2-diglycerides to total diglycerides, acidity, iodine value, and fatty acid composition determined upon analysis of the respective (1)H NMR and (31)P NMR spectra were selected as variables to establish a classification/prediction model by employing discriminant analysis. This model, obtained from the training set of 128 samples, resulted in a significant discrimination among the different classes of oils, whereas 100% of correct validated assignments for 64 samples were obtained. Different artificial mixtures of olive-hazelnut, olive-corn, olive-sunflower, and olive-soybean oils were prepared and analyzed by (1)H NMR and (31)P NMR spectroscopy. Subsequent discriminant analysis of the data allowed detection of adulteration as low as 5% w/w, provided that fresh virgin olive oil samples were used, as reflected by their high 1,2-diglycerides to total diglycerides ratio (D > or = 0.90).
Scientific Opinion on the safety of hemp (Cannabis genus) for use as animal feed
EFSA, Scientific Opinion on the safety of hemp (Cannabis genus) for use as
animal feed, EFSA J. 9 (2011) 1e41.