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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.

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... 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). ...
Article
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.
... 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. ...
Article
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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.
... 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]. ...
Article
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.
... 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. ...
Article
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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
... 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. ...
Article
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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.
... 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]. ...
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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
... 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]. ...
... 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. ...
Article
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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.
... 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. ...
Article
Full-text available
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.
... 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]. ...
Article
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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.
... 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. ...
Article
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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.
... 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. ...
Article
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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.
... 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). ...
Article
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.
... 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. ...
Article
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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.
... 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.
Chapter
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.
Article
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.
Article
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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.
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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.
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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
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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.
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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.