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Chemical characterisation of old cabbage ( Brassica oleracea L. var. acephala ) seed oil by liquid chromatography and different spectroscopic detection systems
Abstract
We report an extensive chemical characterisation of fatty acids, triacylglycerols, tocopherols, carotenoids and polyphenols contained in the oil extracted from old cabbage (Brassica oleracea L. var. acephala) by cold-pressing of the seeds. Analyses were performed by GC-FID combined with mass spectrometry, HPLC with photodiode array, fluorescence and mass spectrometry detection. The 94% of the total fatty acids were unsaturated, rappresented by erucic acid (more than 50%) followed by linoleic, linolenic and oleic acids accounting for approximately 10% each. The most abundant triacylglycerols (>13%) were represented by erucic–gadolenic–linoleic, erucic–eruci–linoleic and erucic–erucic–oleic. Among tocopherols, γ-tocopherol accounted for over 70% of the total content. Thirteen carotenoids and 11 polyphenols were identified and measured. In particular, the total content in carotenoids was 10.9 ppm and all-E-lutein was the main component (7.7 ppm); among polyphenols, six hydroxycinnamic acids and five flavonoids, were identified by combining information from retention times, PDA and MS data.
... The phytochemical screening of B. oleracea L. var. acephala seeds demonstrated the presence of 13 carotenoids, among which all-elutein was the main component [35]. ...
... However, the lack of standards of some compounds is a limiting factor of HPLC viability. Thus, to improve phytochemical detection and quantification, the combination of HPLC with the highly sensitive method MS (LC-MS) is needed as a rapid, selective and sensitive approach [35,115]. Yet, due to its insufficient precision and accuracy to identify some GLS peaks (e.g., similar m/z of both glucoiberin (m/z 422.0255) and gluconasturtiin (m/z 422.0585)) and the lack of reference materials, LC-MS use remains limited [111]. ...
Traditionally, Brassica species are widely used in traditional medicine, human food, and animal feed. Recently, special attention has been dedicated to Brassica seeds as source of health-promoting phytochemicals. This review provides a summary of recent research on the Brassica seed phytochemistry, bioactivity, dietary importance, and toxicity by screening the major online scientific database sources and papers published in recent decades by Elsevier, Springer, and John Wiley. The search was conducted covering the period from January 1964 to July 2022. Phytochemically, polyphenols, glucosinolates, and their degradation products were the predominant secondary metabolites in seeds. Different extracts and their purified constituents from seeds of Brassica species have been found to possess a wide range of biological properties including antioxidant, anticancer, antimicrobial, anti-inflammatory, antidiabetic, and neuroprotective activities. These valuable functional properties of Brassica seeds are related to their richness in active compounds responsible for the prevention and treatment of various chronic diseases such as obesity, diabetes, cancer, and COVID-19. Currently, the potential properties of Brassica seeds and their components are the main focus of research, but their toxicity and health risks must also be accounted for.
... The farmed snails mostly preferred old cabbage until the leaves hardened and only then did they startconsuming other food. It is well known that plants belonging to the same family as old cabbage (Brassicaceae) have high erucic acid content (Mackenzie et al. 1997;Cacciola et al. 2016). Overall, 94% of the total fatty acids in old cabbage were unsaturated, representing more than 50% of the fatty acid composition, followed by the essential FAs, linoleic and linolenic acid (Khan et al. 1985;El-Beltagi et al. 2010;Cacciola et al. 2016). ...
... It is well known that plants belonging to the same family as old cabbage (Brassicaceae) have high erucic acid content (Mackenzie et al. 1997;Cacciola et al. 2016). Overall, 94% of the total fatty acids in old cabbage were unsaturated, representing more than 50% of the fatty acid composition, followed by the essential FAs, linoleic and linolenic acid (Khan et al. 1985;El-Beltagi et al. 2010;Cacciola et al. 2016). On the other hand, the canola oil used in the snail diet had zero percent erucic acid. ...
The fatty acid and mineral matter compositions of the visceral mass and pedal mass of wild and
farmed Cornu aspersum were compared. The relative fatty acid amounts of the visceral and
pedal masses of wild and farmed snails are: polyunsaturated fatty acid (PUFA) > saturated
fatty acid (SFA) > monounsaturated fatty acid (MUFA), PUFA > SFA > MUFA, MUFA > PUFA >
SFA and PUFA > MUFA > SFA, respectively. Wild snails had a higher concentration of iron and
zinc than farmed snails. Selenium was 2.82 times higher in the pedal mass of farmed snails
than the pedal mass of wild snails. Ca:P ratios in the visceral mass of wild snails, visceral
mass and pedal mass of farmed snails were 1.76:1, 1.12:1 and 3.87:1 respectively. Both wild
and farmed snails have high contents of oleic, linoleic, eicosapentaenoic and
docosahexaenoic fatty acids and are a good source of minerals. Careful attention should be
paid, however, as to which diet will be used during farming because the composition of fatty
acid in the snail is affected by diet.
... The farmed snails mostly preferred old cabbage until the leaves hardened and only then did they startconsuming other food. It is well known that plants belonging to the same family as old cabbage (Brassicaceae) have high erucic acid content (Mackenzie et al. 1997;Cacciola et al. 2016). Overall, 94% of the total fatty acids in old cabbage were unsaturated, representing more than 50% of the fatty acid composition, followed by the essential FAs, linoleic and linolenic acid (Khan et al. 1985;El-Beltagi et al. 2010;Cacciola et al. 2016). ...
... It is well known that plants belonging to the same family as old cabbage (Brassicaceae) have high erucic acid content (Mackenzie et al. 1997;Cacciola et al. 2016). Overall, 94% of the total fatty acids in old cabbage were unsaturated, representing more than 50% of the fatty acid composition, followed by the essential FAs, linoleic and linolenic acid (Khan et al. 1985;El-Beltagi et al. 2010;Cacciola et al. 2016). On the other hand, the canola oil used in the snail diet had zero percent erucic acid. ...
The fatty acid and mineral matter compositions of the visceral mass and pedal mass of wild and farmed Cornu aspersum were compared. The relative fatty acid amounts of the visceral and pedal masses of wild and farmed snails are: polyunsaturated fatty acid (PUFA) > saturated fatty acid (SFA) > monounsaturated fatty acid (MUFA), PUFA > SFA > MUFA, MUFA > PUFA > SFA and PUFA > MUFA > SFA, respectively. Wild snails had a higher concentration of iron and zinc than farmed snails. Selenium was 2.82 times higher in the pedal mass of farmed snails than the pedal mass of wild snails. Ca:P ratios in the visceral mass of wild snails, visceral mass and pedal mass of farmed snails were 1.76:1, 1.12:1 and 3.87:1 respectively. Both wild and farmed snails have high contents of oleic, linoleic, eicosapentaenoic and docosahexaenoic fatty acids and are a good source of minerals. Careful attention should be paid, however, as to which diet will be used during farming because the composition of fatty acid in the snail is affected by diet.
... In contrast, experience have shown that green tea [25], caffeine [26] and Aloe Vera [27] are able to reduce oxidative stress. On the other hand, the Mediterranean diet, characterized by vegetables, fruit, cereals, nuts, olive oil and wine consumption is particularly rich in antioxidants [28][29][30][31][32] and molecules of nutritional interest [33][34][35][36]. However, recent studies have shown that, in various populations, the adherence to the traditional Mediterranean diet is decreasing [37,38]. ...
Background and objectives: The aim of this retrospective study was to evaluate the effects of alcohol consumption on oxidative stress. Materials and Methods: The study was conducted by analyzing the increase in lipid peroxidation, the reduction of antioxidant defenses and the alteration of the oxidation/antioxidant balance after the administration of ethanol in 25% aqueous solution (v/v) at a concentration of 0.76 g/kg of body weight daily in two doses for 3 days. The changes in oxidative stress indices were investigated by standard methods previously described. Results: Ethanol administration has determined a significant increase in plasma levels of lipid hydroperoxide (LOOH), malonilaldehyde (MDA) and oxidized glutathione (GSSH), and a decrease in total antioxidant capacity (TAC), reduced glutathione (GSH) and GSH/GSSH ratio. Conclusions: In the proposed experimental condition, the excessive and repeated consumption of ethanol causes oxidative damage, as shown by the increase in lipid peroxidation, the reduction of antioxidant defenses and the alteration of the oxidation/antioxidant balance, which, at least in part, are responsible for the harmful effects of excess ethanol.
... Because these special fatty acids are not present in seed oils from A. thaliana (Li-Beisson et al., 2013), Brassica spp. (Cacciola et al., 2016;Rout et al., 2018;Cartea et al., 2019;Tang et al., 2021), or I. indigotica (Supplemental Figure 16), it remains unclear where and when the genes responsible for ...
Orychophragmus violaceus is a Brassicaceae species widely cultivated in China, particularly as a winter cover crop in northern China due to its tolerance to low temperature and low demand for water. Recently, O. violaceus has also been cultivated as a potential industrial oil seed crop owing to its abundant 24-carbon dihydroxy fatty acids (diOH-FA), which contribute to superior high-temperature lubricant property. In this study, we conducted the de novo assembly of O. violaceus genome. Further whole-genome synteny analysis with the genomes of its relatives demonstrated that O. violaceus is a diploid undergoing an extra whole-genome duplication (WGD) after the Brassicaceae specific α-WGD event, with a basic chromosome number of x = 12. Notably, the formation of diOH-FA is hypothesized to occur after the WGD event. Based on the genome and the transcriptome data of multistage seed development, we predicted that OvDGAT1-1 and OvDGAT1-2 are the candidate genes regulating the storage of diOH-FA in O. violaceus seeds. These results may greatly facilitate the development of heat-tolerant and eco-friendly plant-based lubricants using O. violaceus seed oil as well as improve our understanding of the genomic evolution of Brassicaceae.
... The top 15 Heptacosyl acetate compound acetate is an anti-cause of pain molecular weight 438.77Da. These results were agreed with (Farag et al., 2010) when separating sulfur compounds and antioxidant compounds And anti-cancer of the Crusader family represented by the green faith and the red curse These results were agreed with (Cacciola et al., 2016) when segregating fatty acids and flavonoids from immunity and the results were not fully consistent with ( Hou et al., 2016) Total count of microorganisms Table (3) shows the total number of microorganisms of raw milk treated with cabbage extract. The results of the milk treated with the extract were 0.05% (0.03, 0.022, 0.049, 0.28, 2.3, 34, 52) ×10 6 cfu/ml and for periods (5 hours)-1, 2, 3, 4, 5, 6, 7 days), while the number of microbiological milestones was 0.1% (0.012-0.021, 0.021, 0.045, 0.146, 0.32, 31, 44) × 10 6 cfu / ml and the milk treated at 0.15% 0.009, 0.019, 0.019, 0.4, 13) ×10 6 cfu/ml. ...
The Gas Chromatography/ Mass Spectrometer (GC/MS) method was used to detect the active ingredients in the water extract of the red cabbage and showed several peaks. It was found that most active groups of esters, phenols, Alkanes and carboxylic acids, including (1-octadecene, acid, 5-trime thylsilyl, oxy-methyl ester, 3-Carboxamide, Oxime, 2-trifluoromethylephenyl, Heptacosane, Triacontane and Hexacosane), all of which are antibacterial, different concentrations of water extract of red cabbage were added to raw milk and decreased microbiological numbers increased with concentration for different periods. 0.15% (0.009, 0019, 0.019, 0,039, 0.045, 0.51, 2.4, 13)×10 6 cfu/ mL compared to control treatment (0.03. 0.30, 2.3, 33, 44, 48, 58)×10 6 cfu/ mL For a period of seven days, storage at 4°C , but the molds and yeasts during the seventh day of storage amounted range reached At 0.15 as Log 0.0019, compared to the control treatment it was log 3.7348. The ratio of acidity of raw milk reached 0.19 % and this indicates that the extract of red cabbage increases the shelf life of raw milk.
... The top 15 Heptacosyl acetate compound acetate is an anti-cause of pain molecular weight 438.77Da. These results were agreed with (Farag et al., 2010) when separating sulfur compounds and antioxidant compounds And anti-cancer of the Crusader family represented by the green faith and the red curse These results were agreed with (Cacciola et al., 2016) when segregating fatty acids and flavonoids from immunity and the results were not fully consistent with ( Hou et al., 2016) Total count of microorganisms Table (3) shows the total number of microorganisms of raw milk treated with cabbage extract. The results of the milk treated with the extract were 0.05% (0.03, 0.022, 0.049, 0.28, 2.3, 34, 52) ×10 6 cfu/ml and for periods (5 hours)-1, 2, 3, 4, 5, 6, 7 days), while the number of microbiological milestones was 0.1% (0.012-0.021, 0.021, 0.045, 0.146, 0.32, 31, 44) × 10 6 cfu / ml and the milk treated at 0.15% 0.009, 0.019, 0.019, 0.4, 13) ×10 6 cfu/ml. ...
The Gas Chromatography/ Mass Spectrometer (GC/MS) method was used to detect the active ingredients in the water extract of the red cabbage and showed several peaks. It was found that most active groups of esters, phenols, Alkanes and carboxylic acids, including (1-octadecene, acid, 5-trime thylsilyl, oxy-methyl ester, 3-Carboxamide, Oxime, 2-trifluoromethylephenyl, Heptacosane, Triacontane and Hexacosane), all of which are antibacterial, different concentrations of water extract of red cabbage were added to raw milk and decreased microbiological numbers increased with concentration for different periods. 0.15% (0.009, 0019, 0.019, 0,039, 0.045, 0.51, 2.4, 13)×10 6 cfu/ mL compared to control treatment (0.03. 0.30, 2.3, 33, 44, 48, 58)×10 6 cfu/ mL For a period of seven days, storage at 4°C , but the molds and yeasts during the seventh day of storage amounted range reached At 0.15 as Log 0.0019, compared to the control treatment it was log 3.7348. The ratio of acidity of raw milk reached 0.19 % and this indicates that the extract of red cabbage increases the shelf life of raw milk.
... Hemp (Smeriglio et al., 2016), cabbage (Cacciola et al., 2016) and carrot (Chandra, Kishore, & Ghosh, 2015) all represent sources of bioflavonoids. In vitro and in vivo experiments have demonstrated spasmolytic effects of several bioflavonoids on intestinal motility (Di Carlo, Mascolo, Izzo, & Capasso, 1999;Escobar-Ramos et al., 2017;Gharzouli & Holzer, 2004;Rao et al., 1997) Amira, Rotondo, and Mulè (2008) (Amira et al., 2008) evaluated the impact of several bioflavonoids on the gastric tone in mouse isolated stomachs. ...
G's Formula is a novel equine feed additive formulated to promote optimal GI function. The objective of this study was to determine whether the addition of a simulated digest of the composite feed additive G's Formula (FA) would alter the contractile response of gastric smooth muscle to acetylcholine (Ach). Smooth muscle strips from porcine stomachs were excised and attached to an isometric force transducer. An experiment was run to compare tissue contraction between tissue exposed to FA (FA; n = 8, simulated digest of FA was added to the bath) and control tissue (CO; n = 8, no additions made). Increasing concentrations of Ach were added into the bath such that the concentration increased from 10–8–10−3 M. Based on the analysis of these data, a difference between FA and CO was observed. Therefore, another trial was run which included a blank group (BL n = 6) in which the tissue was exposed to the simulated digest without FA. More CO (n = 5) and FA (n = 4) tissue was also run. Force was compared to baseline and between groups. In FA group, mean force for 1‐min following all Ach additions was higher than baseline (p < .05) and by 2‐min the integral‐under‐force/time curve (AUC) was higher than baseline from 10–7–10−3 M compared to lower concentrations of Ach in both CO (10−6 M for both) and BL (10−5 M and 10−6 M, respectively). By 8‐min AUC of all Ach concentrations were higher than baseline in FA compared to an Ach of 10−6 M in both CO and BL. A simulated digest of FA appears to sensitize gastric smooth muscle to Ach in vitro. FA may increase GI contractility, and the functional effect of this should be studied further in vivo.
... acephala) as an external matrix was applied to determine the recovery of phenols in EVOOs. Cabbage oil was previously analysed to determine if it does not contain the same phenols as olive oils (Cacciola et al. 2016). The extraction procedure was carried out after the addition of known amounts of gallic acid, caffeic acid, ferulic acid, luteolin, oleuropein, apigenin, tyrosol and hydroxytyrosol to the sample chosen for the validation of the extraction method. ...
Extra virgin olive oils (EVOOs) contain various bioactive compounds belonging to phenol family. These compounds are traditionally determined by liquid chromatography, despite such a method implies some issues that have to be taken into account. Therefore, our study was focused on the employment of reversed-phase high-performance liquid chromatography coupled to diode array detection and electrospray ionisation mass spectrometry (RP-HPLC-DAD/ESI-MS) and nuclear magnetic resonance (NMR) approaches, which are here compared in order to provide thorough information about the phenol profile in EVOOs. Data comparison led to matching results with some experimental divergence as expected from a challenging coupled analysis concerning dynamically unstable compounds. Specific concerns of both techniques are described shedding light on the potential advantages arising from the employment of the quick NMR and short and sensitive HPLC analysis. This is the first step toward a joined approach for the future analysis of the phenolic profile.
... Pomegranate mesocarp and exocarp extracts are documented as having anti-inflammatory, antimicrobial and anti-proliferative properties (Viuda-Martos et al. 2010;Duman et al. 2009;Hamad & Al-Momene 2009;Negro et al. 2012;Orgil et al. 2014;Rafiq et al. 2016;Imperatori et al. 2018;Mastrogiovanni et al. 2018;Meselhy et al. 2018;Zhang et al. 2018). The wide range of health-promoting biological activities are related to the presence of bioactive molecules, well represented in nature, comprising anthocyanins, phenolic acids and hydrolyzable tannins (Cacciola et al. 2016;Cicero et al. 2018;Clodoveo et al. 2015;Gervasi et al. 2016). Anthocyanins represent the predominant class of phytochemicals in pomegranate juice, imparting the typical red colour. ...
Punica granatum L., commonly known as pomegranate, is an ancient fruit widely consumed all over the world as fresh fruit or juice. In addition, it is extensively used in therapeutic formulas, cosmetics and food seasonings. The fruit is native to Afghanistan, Iran, China and the Indian sub-continent. The pomegranate market has steadily grown, presumably due to the increasing demand of health-conscious consumers for products with potential beneficial effects on human health, due to the synergistic presence of a unique and complex phytochemical composition that enclose anthocyanins, phenolic acids and hydrolysable tannins. Conventionally, for their analysis liquid chromatography is employed even though it can present some drawbacks in terms of resolving power. In this contribution, as a valuable alternative, comprehensive two-dimensional liquid chromatography with "shifted gradients" in the second dimension, was applied for the characterization of three pomegranate samples, leading to the identification of 37 different polyphenolic compounds.
... [17][18][19] Owing to their effect on health, innovative analyses methods have been used to detect bioactive phenolic compounds in different plant sources. 17,[20][21][22] The aim of the present study was the qualitative and quantitative monitoring of phenolic compounds in PJs obtained from five pomegranates genotypes 'Mollar' (ML), 'Kingdom' (KD), 'Dente di Cavallo' (DC), 'Francofonte' (FR) and 'Santa Tecla' (ST). FR and ST represent two old populations of Sicilian pomegranates. ...
BACKGROUND
Pomegranate fruits are a rich source of polyphenols with numerous health‐promoting effects. Pomegranate juices of five genotypes (“Mollar”, “Kingdom”, “Dente di Cavallo”, and two old populations “Francofonte” and “Santa Tecla”) were evaluated regarding anthocyanin and non‐anthocyanin phenolic contents using UHPLC/Orbitrap‐MS. Moreover total antioxidant activity (TAA) was evaluated using ABTS assay.
RESULTS
23 phenolic compounds were identified. Cyanidin‐3,5‐O‐diglucoside and pelargonidin‐3,5‐O‐diglucoside were the most representative anthocyanins in all genotypes; Santa Tecla population had the highest content of these anthocyanins, 97.64 mg/L and 40.29 mg/L respectively. In Francofonte population, ferulic acid hexoside was the most abundant compound (391.18 mg/L). Total antioxidant activity values ranged between 221.5 and 36.73 μmol Trolox Equivalents/100 ml of juice. High Total Antioxidant Activity (TAA) value was recorded for Santa Tecla pomegranate population.
CONCLUSION
In this paper, UHPLC/Orbitrap‐MS approach was employed, for the first time, to identify the phenolic compound profiling in five pomegranate genotypes. Total antioxidant activity was analyzed using ABTS assay and the results showed a significant variability in nutraceutical potential of studied pomegranate genotypes. The inclusion of phenolic information in the Linear Discriminant Analysis (LDA) allowed reaching very good discriminations among genotypes.
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... Chemical composition together with the contaminant amount investigation is very important for foods characterization (Di Stefano et al. 2014;Mallamace et al. 2014;Naccari et al. 2014;Cicero et al. 2015;Cacciola et al. 2016;Pantano et al. 2016). ...
The aim was to evaluate the susceptibility of bla ESBL producing Enterobacteriaceae to Slovakian Thymus vulgaris essential oil (TVEO) alone and in combination with cefotaxime (CTX). TVEO composition was determined by gas chromatograph-mass spectrometer (GC/MS). Susceptibility to 21 antibiotics was determined by disc diffusion assay. Genes characterization for resistance to β-lactams was accomplished by polymerase chain reaction (PCR). The antibacterial activity was investigated by standard methods. The synergistic interaction was determined by checkerboard test. Thymol (34.5%), p-cymene (22.27%) and linalool (5.35%) were the major components present in the TVEO. The identified strains were multi-drug resistant (MDR). TVEO showed high activity against all MDR strains, including bla ESBL producing isolates, with inhibition zones and MIC values in the range of 24-40 mm/10μL and 2.87-11.5 μg/mL, respectively. TVEO in combination with CTX showed a synergistic action against bla SHV-12 producing Escherichia coli (FICI 0.28) and an additive effect vs ESBL producing Enterobacter cloacae (FICI 0.987).
... The Mediterranean diet is a source of healthy constitutes such as grains, cereals, legumes, fresh fruits, vegetables, dried fruits, olive oil, spices and wine. As reported by several authors, the chemical fingerprinting of these food matrices has a key role to guarantee their genuineness and traceability Mallamace et al. 2014;Tuttolomondo, Dugo, Ruberto et al. 2015;Cacciola et al. 2016;Cannas et al. 2016;Corsaro et al. 2016;Gervasi et al. 2016;Albergamo et al. 2017). The opportunity of avoiding the use of chemicals on field by using natural compounds to control weed for foodstuff cultivated would benefit to the food risk assessment (Cimmino et al. 2012). ...
Breakfast habits affect the nutritional status and health of people, in particular children and adolescents. This is the second part a previous study about the adherence to the Mediterranean diet in a Sicilian (Italy) student population. The investigation analysed both normal weight and overweight subjects in order to understand how eating habits, number of meals and daily calorie intakes could affect their body mass indexes (BMI). The aim of this second part was to analyse the breakfast nutritional profiles of this student population. The results highlighted that breakfast was regularly consumed by a percentage ranging from a maximum of 84% (in normal subjects) to a minimum value of 57.4% (in overweight/obese students). Milk, yoghurt, sugar, bread/rusk and tea contributed as main foods to the breakfast composition. The results highlighted that subjects who consumed breakfast showed lower BMI values with significant differences between normal and overweight/obese students.
... Olive oil is the most important food of the Mediterranean diet. Also the beneficial properties and characteristics of all the Mediterranean key foods have been investigated Mallamace et al. 2014;Cicero et al. 2015;Clodoveo et al. 2015;Corsaro et al. 2015;Dugo et al. 2015;Bua et al. 2016;Corsaro et al. 2016;Cacciola et al. 2016;Gervasi et al. 2016;Pantano et al. 2016;Albergamo et al. 2017;Mallamace et al. 2017;Mottese et al. 2017;Salvo et al. 2017aSalvo et al. , 2017b. ...
Since the last decades, socio-economic changes have a key role on eating habits affecting the nutritional status and health of people, in particular children and adolescents. The aim of this study was to compare the diet of student population both normal weight and overweight and obese in order to understand their eating habits by comparing the different diets of the student referring to the Mediterranean diet. The study comprised 337 Sicilian students aged 9 to 13 years, 96 in primary schools and 241 in secondary schools, respectively, in three Sicilian cities namely, Messina, San Piero Patti and Ragusa. The variables studied were height, weight, body mass index (BMI) and adherence to the Mediterranean Adequacy Index (MAI) diet quality indicator. Interestingly, the results highlighted 2.67 MAI mean value for normal weight students while 1.27 MAI mean value indicating a decreased adherence to the Mediterranean diet in overweight students.
... Previous works analysed the nutritional value of many Brassicaceae plants mainly considering the phytochemical composition of seed oil (Cacciola et al. 2016), leaves or other edible portions in fresh tissues, or after cooking or storing (Korus and Lisiewska 2011;Bongoni et al. 2014). ...
We report the spectrophotometric determination of total polyphenols, flavonoids, glucosinolates and antioxidant activity in seeds, seedlings and leaves of Tuscan black kale. The highest content of phytochemicals was observed in 10 days sprouts and antioxidant activity was maximum in 2, 4 days seedlings. Identification and characterisation of phytochemicals were performed by mass spectrometry (MS), high resolution and tandem MS with electrospray ionisation mode. Low-molecular-weight metabolites were evidenced in seeds while metabolites at high m/z range were detected in cotyledons and leaves. MS spectra evidenced different phenolic compounds (flavonoid caffeoyl glucose, hydroxycinnamic acid sinapine) and glucosinolates (glucoerucin, glucobrassicin and glucoraphanin) in function of developmental stage; galactolipids ω3 and ω6 were observed in leaves. Identification of stages with the highest phytochemicals content encourages the consumption of black kale sprouts and young leaves. Our research can support food and pharmaceutical industries for production of health promoting products from black kale.
... In modern life, they result to be very interesting molecules as nutraceuticals and functional foods (Lesschaeve & Noble 2005;Scalbert et al. 2005;Spencer et al. 2008;Alesci et al. 2014;Corsaro et al. 2015;Soares et al. 2015;Cacciola et al. 2016). ...
... Polyphenols are secondary metabolites commonly found in food and waste derived from plants (Alesci et al. 2014;Cacciola et al. 2016;Gervasi et al. 2016). In line with literature, globe artichoke head demonstrated to be a valuable source of two phenolic classes, namely flavonoids and caffeic acid derivatives, contributing considerably to its nutraceutical value, due to a well-know therapeutic activity (Pandino et al. 2011a;Lombardo et al. 2010Lombardo et al. , 2009Fratianni et al. 2007). ...
Globe artichoke has been long considered a nutraceutical food for its valuable content of bioactive compounds. However, beside a well known polyphenol profile, poor information is available about its metabolite and mineral composition. The aim of this study was to investigate edible parts of Sicilian artichokes, ‘Spinoso di Menfi’ and ‘Violetto di Niscemi’, by 1H NMR and ICP-MS for elucidating these
compositional aspects. Although bracts and hearts of both artichokes shared a very similar metabolite pattern, ‘Spinoso di Menfi’ showed a higher number of metabolites, such as amino acids and polyphenols,
than ‘Violetto di Niscemi’. ‘Spinoso di Menfi’ was also marked by higher levels of macro- and microelements when compared to ‘Violetto di Niscemi’. Also, artichoke heart demonstrated to accumulate higher mineral levels than bracts. 1H NMR and ICP-MS successfully profiled metabolites and metals in such plant food, partially covering the lack of literature data about ‘Spinoso di Menfi’ and ‘Violetto di Niscemi’ artichokes.
... Seeds from Brassica species are known to produce fatty acids, triacylglycerols, tocopherols, carotenoids, polyphenols and glucosinolates (GLs) (Liang et al. 2013; Cacciola et al. 2016). endemic to eastern Europe including Croatia (Horn & Vaughan 1983; Warwick & Francis 1994). ...
The glucosinolates (GLs) present in seed extracts of Brassica elongata Ehrh., B. botteri Vis and B. cazzae Ginzb. & Teyber from Croatia were identified by LC–MS. 4-Hydroxyindol-3-ylmethyl GL (3) was the major GL in the seeds of B. elongata, along with the four minor GLs 2-(R)-hydroxy-3-butenyl- (1), 3-butenyl- (2), 4-pentenyl- (4) and indol-3-ylmethyl (5). The seeds of B. botteri (Vis island) and B. cazzae (Sušac island) contained 2 as the major GL as well as 1, 3, 5 and 4-methoxyindol-3-ylmethyl GL (6). However, the GLs in B. botteri (Palagruža island) differed from other varieties having 2-propenyl GL (7) as the major GL in the seeds, and the four minor GLs 2, 3, 5 and 6. This first report of the GL content in the seeds of B. elongata, B. botteri and B. cazzae indicates that the unique GL profiles could be specific to the geographical origin of the plant.
... Pistacia vera L. belonging to the Anacardiaceae family, is a small tree originally from Central Asia and the Middle east (Monastra et al. 1987). The Mediterranean basin around the etna volcano is ideal for the cultivation of vegetable products and different studies on chemical characterisation of typical sicilian products have been conducted (Mallamace et al. 2014;Cicero et al. 2015;Corsaro et al. 2015;Dugo et al. 2015;Salvo et al. 2015;Tuttolomondo et al. 2015;Cacciola et al. 2016). A high quality pistachio cultivar, which represents the 80% of the Italian production, is produced in Bronte (Sicily). ...
A gas chromatographic with flame ionization detector (GC-MS FID) method for the identification and quantification of fatty acids based on the extraction of lipids and derivatisation of free acids to form methyl esters was developed and validated. The proposed method was evaluated to a number of standard FAs, and Bronte pistachios samples were used for that purpose and to demonstrate the applicability of the proposed method. In this regard, repeatability, mean and standard deviation of the analytical procedure were calculated. The results obtained have demonstrated oleic acid as the main component of Bronte pistachios (72.2%) followed by linoleic acid (13.4%) and showed some differences in composition with respect to Tunisian, Turkish and Iranian pistachios.
... In modern life, they result to be very interesting molecules as nutraceuticals and functional foods (Lesschaeve & Noble 2005;Scalbert et al. 2005;Spencer et al. 2008;Alesci et al. 2014;Corsaro et al. 2015;Soares et al. 2015;Cacciola et al. 2016). ...
In 2011 vintage, the evolution of monomer and total anthocyanins, as well as of total flavonoids and polyphenols of grapes and wine of Nero d'Avola and Perricone, varieties cultivated in Sicily, was studied. Anthocyanin profiles are commonly used for grapevine cultivar identification because it is currently accepted that this trait is closely related to their genetic characteristics. The concentration of Nero d'Avola and Perricone anthocyanins was determined by HPLC-DAD.
Olea europaea, meaning "European olive", is a small tree belonging to the family Oleaceae, occurring in the Mediterranean Basin. Olive oil is an essential component of an equilibrated diet because of its nutritional value. Among micronutrients, phenolic compounds did show important beneficial effects for human health. The majority of the research studies on the phenol content are carried out by liquid chromatography combined to photodiode array and/or mass spectrometry detection; however, because of matrix complexity, one‐dimensional liquid chromatography cannot be sometimes sufficient to obtain rewarding separations, requiring more advanced analytical techniques. In this work, comprehensive two‐dimensional liquid chromatography, incorporating RP‐Amide and C18 stationary phases, in the first and second dimension, respectively, both under reversed phase conditions, was investigated for the determination of the phenolic fraction in extra virgin olive oil samples. As far as detection is concerned, triple quadrupole mass spectrometry was employed under multi reaction monitoring mode offering superior selectivity and sensitivity. The reduction of matrix effects, when using LC × LC with respect to conventional 1D‐LC, was assessed by comparing the slopes of calibration curves built from standard solutions and spiked olive oil samples.
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Two new phenolic glycoside compounds (1, 2) and ten known analogues (3−12) have been isolated from the ethanolic extract of Brassica rapa flowers and identified as 2-O-β-d-glucopyranosyl-(1S)-(4-methoxyphenyl)ethylene glycol (1), 2-(4-O-β-d-allopyranosyl)phenyl-ethanol (2), 2-O-β-d-glucopyranosyl-(1S)-phenylethylene glycol (3), 2-O-β-d-glucopyranosyl-(1R)-phenylethylene glycol (4), (Z)-p-coumaryl-O-β-d-glucopyranoside (5), phenyl-O-β-d-glucopyranoside (6), 2-phenylethyl-O-β-d-glucopyranoside (7), salidroside (8), 2-(2-hydroxyphenyl)ethanol-O-β-d-glucopyranoside (9), 4-methoxybenzyl-O-β-d-glucopyranoside (10), 2,4,6-trimethoxyphenyl-1-O-β-d-glucopyranoside (11) and sachaliside 1 (12). The structures of 1 and 2, including absolute configurations, were determined by spectroscopic data (¹H NMR, ¹³C NMR, HSQC, HMBC and ORD) and chemical methods. In addition, most of them exhibited inhibitory activity with IC50 values ranging from 14.43 to 50.20 μM in comparison to the positive control acarbose (IC50 = 15.76 μM) in intestinal α-glucosidase inhibitory activity tests.
Eruca sativa and Brassica juncea belong to the Brassicaceae family and have been used traditionally for the treatment of cancer and various cardiovascular ailments. A rapid and simple ultra performance liquid chromatography (UPLC) method has been developed for the simultaneous quantification of erucin, allyl isothiocyanate and benzyl isothiocyanate in E. sativa and B. juncea oil. Eruca sativa oil contains erucin (28.93%), allyl isothiocyanate (0.06%) and benzyl isothiocyanate (0.70%). Identification of other secondary metabolites in E. sativa and B. juncea oil and aqueous methanolic extracts were also carried out using ultra performance liquid chromatography-electro spray ionization-quadrupole time of flight (UPLC-ESI-QTOF). The UPLC-ESI-QTOF based study leads to the identification of ten compounds in B. juncea oil and three compounds in E. sativa oil. The UPLC-ESI-QTOF analysis of aqueous methanolic extracts of E. sativa and B. juncea leads to the identification of eight and nine compounds, respectively.
Samples of the selected red wine varieties grown in Montenegro (Merlot, Cabernet Sauvignon and Vranac; vintages 2010–2012) were compared according to total phenolic content, anti-DPPH radical activity, phenolic profile and elemental composition. All the samples showed profound anti-DPPH radical activity, due to high content of total phenolic compounds (R = 0.92). The most abundant phenolics were catechin and gallic acid with the highest values recorded for Merlot 2012 (43.22 and 28.65 mg/L, respectively). In addition to this, the content of essential elements including the potentially toxic ones was within healthy (safe) level for all the samples analysed. This study has actually pointed out Merlot wine variety as the best quality one, though all three varieties may be used as safe and health-promoting nutritional products.
Owing to sulforaphane presence, a dietary consumption of Brassicaceae prevents chronic diseases. This hormetic compound induces adaptive stress response at subtoxic doses, while doses that exceed the cellular defence are toxic. In HepG2, Caco-2 and Vero cells, we investigated the sulforaphane (SFN) (5 μM) role in counteracting redox imbalance induced by VOSO4 [V(IV)]. 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) test showed a dose-dependent viability reduction (r < -0.95; p < 0.01) (range 5-80 μM). At 5 μM, SFN enhancement of mitochondrial activity was confirmed by Δψm (p < 0.05) both in basal condition and in redox-stressed cells. Intracellular ROS, DNA and lysosomal oxidative damages underlined the indirect antioxidant SFN activity, confirmed by the increase of GSH. The SFN empowering effects on mitochondrial function were imputable to the presence of mitochondrial proteins among the Nrf2-responsive phase II proteins. Considering the link between oxidative stress and chronic diseases, a long-term dietary intake of Brassicaceae could be strongly advisable.
The ever-increasing problem of pancreatitis due to alcohol abuse demands evaluation of novel drugs of plant origin. This study explores the therapeutic effects of the methanolic extract of Brassica oleraceae (MEBO) on ethanol and cerulein induced pancreatitis in rats. The MEBO was subjected to GC-MS and HPLC analysis. Male albino Wistar rats were divided into various groups, fed with alcohol (36% of total calories for 5 weeks) and cerulein (20 μg/kg b.wt i.p, weekly thrice for last three weeks) with or without MEBO (40 mg/kg b.wt). Serum lipase, amylase, IL-1β, IL-18, caspase-1, lipid peroxides, oxidative stress index and antioxidant status were assessed in pancreas. Six compounds were identified in GC-MS analysis. Co-administration of MEBO reduced the pancreatic marker enzymes in serum, IL-1β, IL-18 and caspase-1 and increased the antioxidant status of pancreas. The pancreato-protective effect of Brassica oleraceae may be attributed to well-known anti-inflammatory flavonoids, luteolin, quercetin and myricetin.
Vegetable oils are the richest dietary sources of vitamin E. Vitamin E determination levels in foods are of great importance to adjust the ingestion of nutrients by the population. The purpose of this paper is to determine the concentration of alpha-tocopherol and gamma-tocopherol in vegetable oils and compare the alpha-tocopherol value to the nutritional requirement of vitamin E. The analysis was performed using High Performance Liquid Chromatography. The values expressed as mg/kg for alpha and gamma-tocopherol were, respectively, 120.3 +/- 4.2 and 122.0 +/- 7.9 in canola oil; 432.3 +/- 86.6 and 92.3 +/- 9.5 in sunflower oil; 173.0 +/- 82.3 and 259.7 +/- 43.8 in corn oil; 71.3 +/- 6.4 and 273.3 +/- 11.1 in soybean oil. A significant difference was encountered between the alpha-tocopherol concentrations in vegetable oils. Similar results were found for gamma-tocopherol, except for corn and soybean oils. It was concluded that the soybean oil was not considered a source of vitamin E. The canola and corn oils were considered sources, and the sunflower oil was considered an excellent source.
In this study the chemical characterisation of 10 Sicilian Rosmarinus officinalis L. biotypes essential oils is reported. The main goal of this work was to analyse the relationship between the essential oils yield and the geographical distribution of the species plants. The essential oils were analysed by GC-FID and GC-MS. Hierarchical cluster analysis and principal component analysis statistical methods were used to cluster biotypes according to the essential oils chemical composition. The essential oil yield ranged from 0.8 to 2.3 (v/w). In total 82 compounds have been identified, these represent 96.7-99.9% of the essential oil. The most represented compounds in the essential oils were 1.8-cineole, linalool, α-terpineol, verbenone, α-pinene, limonene, bornyl acetate and terpinolene. The results show that the essential oil yield of the 10 biotypes is affected by the environmental characteristics of the sampling sites while the chemical composition is linked to the genetic characteristics of different biotypes.
In this study the agronomical and chemical characterization of 13 Sicilian biotypes of Thymbra capitata (L.) Cav., grown under the same agricultural and environmental condition, are reported. The main morpho-productive parameters and quali-quantitative profile of essential oils were determined. The essential oils were analyzed by GC-FID and GC-MS. Hierarchical Cluster Analysis and Principal Component Analysis statistical methods were used to group biotypes according to the essential oils chemical composition. The essential oil yield ranged between 4.6 and 8.1 (v/w).
38 essential oil compounds have been identified. The compounds mostly represented were: α-Pinene, Myrcene, α-Terpinene, p-Cymene, γ-Terpinene, Borneol, Carvacrol and β-Caryophyllene. In all biotypes the Carvacrol (67.4-79.5%) was the main compound, confirming that Thymbra capitata is a carvacrol chemotype. The results showed that all Sicilian Thymbra biotypes have a good adaptation to the climatic conditions of the test environment.
In this work, ultra high performance liquid chromatography was used for the characterization of non polar lipids (triacylglycerols) in milk samples of different origin, as well as milk-derivatives. For tackling such a task, three core-shell type octadecylsilica columns were serially coupled, reaching a total stationary phase length of 45cm, using acetonitrile-isopropanol gradient elution allowing triacylglicerol separation according to increasing partition number. The employment of an ion-trap-time-of-flight detection in conjunction with atmospheric-pressure chemical ionization mass spectrometry was carried out to positively identify a number of 243 different triacylglycerols containing up to 22 fatty acids, with 2-22 carbon atom alkyl chain length, and 0-3 double bonds. This work reports an extensive characterization of the triacylglycerol fraction in milk and milk-related samples of different sources.
Oilseed samples from four Acacia species ( A. cyclops, A. ligulata, A. salicina and A. cyanophylla) were analyzed in order to evaluate the potential nutritional value of their unexploited seeds.
Samples were collected from different Tunisian geographic locations. Seed oils were extracted and carotenoids, tocopherols and sterols were analyzed using chromatographic methods.
The studied Acacia seeds seem to be quite rich in lipids (from 6% to 12%). All Acacia species contain mainly the xanthophylls zeaxanthin and lutein compounds: from ca. 38 mg.kg-1 of total lipids (A. cyclops) to ca. 113 mg.kg-1 of total lipids (A. cyanophylla). Total tocopherols varied from ca. 221 mg.kg-1 of total lipids (A. cyclops) to ca. 808 mg.kg-1 of total lipids (A. ligulata). Sterols are highly present and their contents ranged between ca. 7 g. kg-1 of total lipids (A. salicina) and 11 g. kg-1 of total lipids (A. cyclops).
This study highlights that these unexploited seeds might have a potential nutritional value and encourages researchers to more explore and find developments for these plants for healthy purposes.
Two population-based, case-control studies have documented reduced risk of prostate cancer in men who consume cruciferous vegetables. Cruciferae contain high levels of the isothiocyanate sulforaphane. Sulforaphane is known to bolster the defenses of cells against carcinogens through up-regulation of enzymes of carcinogen defense (phase 2 enzymes). Prostate cancer is characterized by an early and near universal loss of expression of the phase 2 enzyme glutathione S-transferase (GST)-pi. We tested whether sulforaphane may act in prostatic cells by increasing phase 2 enzyme expression. The human prostate cancer cell lines LNCaP, MDA PCa 2a, MDA PCa 2b, PC-3, and TSU-Pr1 were treated with 0.1-15 microM sulforaphane in vitro. LNCaP was also treated with an aqueous extract of broccoli sprouts. Quinone reductase enzymatic activity, a surrogate of global phase 2 enzyme activity, was assayed by the menadione-coupled reduction of tetrazolium dye. Expression of NQO-1, GST-alpha, gamma-glutamylcysteine synthetase-heavy and -light chains, and microsomal GST was assessed by Northern blot analysis. Sulforaphane and broccoli sprout extract potently induce quinone reductase activity in cultured prostate cells, and this induction appears to be mediated by increased transcription of the NQO-1 gene. Sulforaphane also induces expression of gamma-glutamylcysteine synthetase light subunit but not the heavy subunit, and this induction is associated with moderate increases in intracellular glutathione levels. Microsomal and alpha-class glutathione transferases were also induced transcriptionally. Sulforaphane induces phase 2 enzyme expression and activity significantly in human prostatic cells. This induction is accompanied by, but not because of, increased intracellular glutathione synthesis. Our findings may help explain the observed inverse correlation between consumption of cruciferae and prostate cancer risk.
Tocochromanols encompass a group of compounds with vitamin E activity essential for human nutrition. Structurally, natural vitamin E includes eight chemically distinct molecules: alpha-, beta-, gamma- and delta-tocopherol; and alpha-, beta-, gamma- and delta-tocotrienol. Symptoms caused by alpha-tocopherol deficiency can be alleviated by tocotrienols. Thus, tocotrienols may be viewed as being members of the natural vitamin E family not only structurally but also functionally. Palm oil and rice bran oil represent two major nutritional sources of natural tocotrienol. Taken orally, tocotrienols are bioavailable to all vital organs. The tocotrienol forms of natural vitamin E possesses powerful hypocholesterolemic, anti-cancer and neuroprotective properties that are often not exhibited by tocopherols. Oral tocotrienol protects against stroke-associated brain damage in vivo. Disappointments with outcomes-based clinical studies testing the efficacy of alpha-tocopherol need to be handled with caution and prudence recognizing the untapped opportunities offered by the other forms of natural vitamin E. Although tocotrienols represent half of the natural vitamin E family, work on tocotrienols account for roughly 1% of the total literature on vitamin E. The current state of knowledge warrants strategic investment into investigating the lesser known forms of vitamin E.
More than twenty years after the idea of this Carotenoids book series was first discussed, we finally reach the end of the project with Volume 5, which covers the functions and actions of carotenoids in human nutrition and health. In 1971, in Isler’s book Carotenoids, functions of carotenoids and vitamin A were covered in just two chapters. Now, thanks to technical developments and multidisciplinary approaches that make it possible to study functional processes in great detail, this subject is the most rapidly expanding area of carotenoid research, and occupies two full volumes, Volumes 4: Natural Functions and 5: Nutrition and Health. Although Volume 5 can be used as a single stand-alone volume, the two were planned as companion volumes to be used together. To understand the mechanisms of functions and actions of carotenoids, including how carotenoids may be involved in maintaining human health, requires understanding of the underlying principles, which are presented in the first part of Volume 4. The general philosophy and strategy of the series, to have expert authors review and analyse critically a particular topic and present information and give guidance on practical strategies and procedures is maintained in Volumes 4 and 5. It is also the aim that these publications should be useful for both experienced carotenoid researchers and newcomers to the field.
The 12th International Symposium on Plant Lipids was held at the University of Toronto, Canada, from July 7th to 12th, 1996. The conference was attended by over 200 scientists from university, government and corporate laboratories from 24 different countries. The topics covered in the symposium ranged from basic physiology, biochemistry and molecular biology of plant lipids to transformation and genetic engineering of crop plants. Oil seed plants were a particular focus of the symposium. There were 62 oral and 96 posters presentations. A special lecture in memory of the founder of this series of symposium, Terry Galliard, was presented by John Shanklin. This Proceedings Book has been dedicated to Grattan Roughan for his important contributions to our knowledge of plant lipid metabolism. This volume contains manuscripts submitted from most of the presentations at the symposium. It provides a useful summary of the major fields of plant lipid studies and our present state of knowledge. The papers are arranged in eight sections covering the major areas in the field of plant physiology, biochemistry and molecular biology of plant lipids. We would like to thank Valerie Imperial, Rajesh Khetarpal and Mary Williams for their invaluable help in organizing and running the meetings and excursions. John P. Williams, Mobashsher U. Khan and Nora W. Lem Toronto, Canada, October 1996 xvii DEDICATION This volume is dedicated to Grattan Roughan.
Erucic acid is generally excluded from the sn-2 position of seed oil triglycerides (TAGs)of Brassicacea species. Stereospecific analyses of Brassicajuncea, B. napus, B. oleracea, B. rapa, Crambe abyssinica, Lunaria annua, Sinapis alba, and other wild Cruciferae (1–4) have not yet detected significant amounts of erucic acid in the sn-2 position.
High resolution Nuclear Magnetic Resonance (NMR) spectroscopy is a very powerful tool for comprehensive food analyses and especially for Extra-Virgin Olive Oils (EVOOs). We use the NMR technique to study the spectral region of aldehydes (8–10 ppm) for EVOOs coming from the south part of Italy. We perform novel experiments by using mono and bidimensional band selective spin-echo pulse sequences and identify four structural classes of aldehydes in EVOOs. For the first time such species are identified in EVOOs without any chemical treatment; only dilution with CDCl3 is employed.
This would allow the discrimination of different EVOOs for the aldehydes content increasing the potentiality of the NMR technique in the screening of metabolites for geographical characterization of EVOOs.
In this research a comparative sensory evaluation was carried out among typical fish from the strait of messina. The fish were caught between march and july 2009 between cape peloro and cape s. Raineri. Bogue (boops boops) and horse mackerel (trachurus trachurus) were compared with swordfish (xiphias gladius). The sensory characteristics of these fishes were evaluated in relation to their fatty acid profile.
In this work the characterisation of the lipid fraction of several species of marine macro algae gathered along the eastern coast of Sicily is reported. Two species of green marine algae (Chloropyceae), two species of red marine algae (Rhodophyceae) and four species of brown marine algae (Pheophyceae) were evaluated in terms of fatty acids, triacylglycerols, pigments and phospholipids profile. Advanced analytical techniques were employed to fully characterise the lipid profile of these Mediterranean seaweeds, such as GC-MS coupled to a novel mass spectra database supported by the simultaneous use of linear retention index (LRI) for the identification of fatty acid profile; LC-MS was employed for the identification of triacylglycerols (TAGs), carotenoids and phospholipids; the determination of accurate mass was carried out on carotenoids and phospholipids. Quantitative data are reported on fatty acids and triacylglycerols as relative percentage of total fraction.
A non-aqueous reversed phase high performance liquid chromatography method was developed, and optimized for triacylglycerol analysis in a Brevoortia tyrannus (menhaden) oil sample. Four columns were serially coupled to tackle such a task, for a total length of 60cm of shell-packed stationary phase, and operated under ultra high pressure conditions. As detection, positive-ion atmospheric pressure chemical ionization mass spectrometry was used to attain identification of the analyzed sample components. A number of 137 triacylglycerols containing up to 19 fatty acids, with 14-22 carbon atom alkyl chain length and 0-6 double bonds, were positively identified in the complex lipidic sample. This is the first work that reports an extensive characterization of the triacylglycerol fraction of menhaden oil.
The analytical benefits of automated comprehensive two-dimensional chromatographic methods have been exploited and emphasized by part of the chromatographic community, particularly in the past decade. The most important novelty of comprehensive multidimensional (MD) techniques, with respect to classical MD chromatography, is that the entire injected sample is subjected to two independent separation processes, thus greatly enhancing peak capacity. The unsuspectedly complex nature of many real-world samples has been elucidated through the enhanced resolving power of these techniques.The present review reports on the employment of comprehensive chromatographic methods [based on gas chromatography (GC), liquid chromatography (LC), LC-GC and packed supercritical fluid chromatography (pSFC)] in the field of lipid analysis. We also give brief information on the history and the state-of-the-art of the most widely-used techniques.
In this article, a novel and efficient analysis method is described to simultaneously and quantitatively determine glucoraphanin and its major degradation product sulforaphane by reversed-phase high-performance liquid chromatography (HPLC) coupled with an evaporative light-scattering detector (ELSD). This method was validated according to the regulatory guidelines with respect to precision, accuracy and linearity. The HPLC-ELSD method was successfully used to assess the contents of glucoraphanin and sulforaphane in varieties of Brassica oleracea seeds. The developed analytical method not only avoids the underestimation of total glucoraphanin content, but also provides a reduction in analysis time and good efficiency and sensitivity compared to with conventional HPLC methods.
A chemical characterization of the major components, namely, triacylglycerols (TAGs), polyphenols, and tocopherols in a Sacha inchi oil derived from cold pressing of the seed, is hereby reported. To tackle such a task, high-performance liquid chromatography in combination with photodiode array (PDA), fluorescence (RF), and mass spectrometry (MS) detection was employed. The latter was interfaced with atmospheric pressure chemical ionization and with electrospray ionization for the analysis of TAGs and polyphenols, respectively, whereas RF detection was tested for the determination of tocopherol content. Furthermore, fatty acid methyl esters (FAMEs) were evaluated by gas chromatography-flame ionization detector. A 93% amount of total fatty acids was represented by unsaturated FAMEs with the greatest percentage represented by linoleic (L) and linolenic (Ln) accounting for approximately 50 and 36%, respectively. The main TAGs (>10%) were represented by LLnL, LnLnLn, and LnLLn; the latter was present in the oil sample at the highest percentage (22.2%). Among tocopherols, γ-tocopherol was detected to be the most abundant component (over 50%). The polyphenolic composition was also investigated, and a total of 15 compounds were positively identified, through the complementary analytical information coming from PDA and MS data. To the best of our knowledge, this is the first report providing a thorough chemical characterization of a Plukenetia volubilis L. oil.
An optimized 2-D liquid chromatography (LC×LC) set-up, based on the different selectivities of a silver ion (Ag) and a non-aqueous reversed phase (NARP), employed in the first (D1) and the second dimension (D2), respectively, in combination with evaporative light-scattering detection (ELSD), has been developed for the analysis of the triacylglycerol (TAG) fraction in a Borago officinalis oil. The 2-D set-up, thanks to the complementary separation selectivity provided by the two columns, allowed to distribute 78 TAGs throughout the 2-D LC retention plane otherwise unachievable by 1-D LC.
The present research is focused on the GC-FID determination of fatty acid methyl esters (FAMEs) in diesel blends, by means of an ionic liquid stationary phase, characterized by a dicationic 1,9-di(3-vinyl-imidazolium)nonane bis(trifluoromethyl)sulfonylimidate structure (SLB-IL100). The high polarity of the ionic liquid stationary phase allowed the separation of the FAMEs, from the less-retained hydrocarbons, thus avoiding the requirement of a hydrocarbon LC pre-separation. The results derived from the analyses of a soybean FAMEs B20 sample, carried out on an SLB-IL100 conventional column (30 m x 0.25 mm i.d. x 0.20 mm d(f)), were compared with those attained on a polyethylene glycol column, of equivalent dimensions. Conventional and fast GC methods, for the analysis of FAMEs in diesel blends, were developed on an SLB-IL100 30 m x 0.25 mm i.d. x 0.20 microm d(f) and on an SLB-IL100 12 m x 0.10 mm i.d. x 0.08 microm d(f) column, respectively. The optimized IL methods were subjected to validation: retention time and peak area intra-day precision (n=5) were good, with CV % values lower than 0.08% and 4.9%, respectively. With regards to the quantitation of FAMEs in biodiesel blends, a five points calibration curve was constructed, using C(17:0) as internal standard.
The present research is focused on the evaluation of one 0.10 mm i.d. and two 0.25 mm i.d., ionic liquid (IL) stationary phase [1,9-di(3-vinyl-imidazolium) nonane bis(trifluoromethyl) sulfonyl imidate] columns, with lengths of 12 (the microbore capillary), 30 and 100 m, in the GC analysis of cis/trans fatty acid methyl esters (FAMEs). The selectivity of the IL columns toward a series of standard C(18:1), C(18:2), and C(18:3) geometric isomers (a group of 22 compounds was subjected to GC analysis) was compared to the performance of a widely used column in the cis/trans FAMEs analysis field, viz., a 100 m x 0.25 mm i.d. capillary with a 0.20 microm stationary phase film of bis-cyanopropyl polysiloxane (SP-2560). The selectivity provided by the IL phase was superior if compared to that of the other well-established capillary. An optimized IL method, using the longer column, was subjected to validation: retention time and peak area intraday precision (n = 5) were good, with RSD values lower than 0.07% and 6.6%, respectively; LODs (considering a S/N of 3) for C(18:1Delta)(9tr) and C(18:2Delta)(9tr,12tr) were 0.15 (7.3 ppm) and 0.18 ng (9.1 ppm) on-column, respectively, while LOQs (considering a S/N of 10) were 0.49 (24.3 ppm) and 0.60 ng (30.2 ppm), respectively; the method was found to be linear, for both trans FAMEs, in the 10-2000 ppm range. For the evaluation of accuracy, a hydrogenated margarine, spiked with known amounts of C(18:3Delta)(9c,12c,15c), was subjected to analysis using C(13:0) as an internal standard.
Kale is a leafy green vegetable belonging to the Brassicaceae family, a group of vegetables including cabbage, broccoli, cauliflower, and Brussels sprouts, with a high content of health-promoting phytochemicals. The flavonoids and hydroxycinammic acids of curly kale ( Brassica oleracea L. ssp. oleracea convar. acephala (DC.) Alef. var. sabellica L.), a variety of kale, were characterized and identified primarily through HPLC-DAD-ESI-MS(n) analysis. Thirty-two phenolic compounds including glycosides of quercetin and kaempferol and derivatives of p-coumaric, ferulic, sinapic, and caffeic acid were tentatively identified, providing a more complete identification of phenolic compounds in curly kale than previously reported. Moreover, three hydroxycinnamic acids and one flavonoid with an unusual high grade of glycosylation, quercetin-3-disinapoyl-triglucoside-7-diglucoside, have been tentatively identified for the first time. The influence of different extraction conditions (extraction method, solvent type, solvent/solid ratio, and duration of extraction) was investigated. The total flavonol and hydroxycinnamic acid contents in curly kale determined as rutin equivalents (RE) were 646 and 204 mg of RE/100 g of fresh weight (fw), respectively. The contents of individual flavonoids ranged from 2 to 159 mg of RE/100 g of fw, with main compounds kaempferol-3-sinapoyl-diglucoside-7-diglucoside (18.7%) and quercetin-3-sinapoyl-diglucoside-7-diglucoside (16.5%). After acidic hydrolysis, two flavonol aglycones were identified in curly kale, quercetin and kaempferol, with total contents of 44 and 58 mg/100 g of fw, respectively.
The main constituents of plant oils are complex mixtures of TGs differing in acyl chain lengths, number and positions of double bonds, and regioisomerism. A non-aqueous reversed-phase HPLC method with acetonitrile-2-propanol gradient and 30 + 15 cm NovaPak C18 columns makes possible an unambiguous identification of the highest number of TGs ever reported for these oils, based on positive-ion APCI mass spectra. A new approach to TG quantitation is based on the use of response factors with three typical detection techniques for that purpose (APCI-MS, evaporative light-scattering detection, and UV at 205 nm). Response factors of 23 single-acid TGs (saturated TGs from C7 to C22, 7 unsaturated TGs), 4 mixed-acid TGs, diolein and monoolein are calculated from their calibration curves and related to OOO. Due to differences between saturated and unsaturated acyl chains, the use of response factors significantly improves the quantitation of TGs. 133 TGs containing 22 fatty acids with 8-25 carbon atoms and 0-3 double bonds are identified and quantified in 9 plant oils (walnut, hazelnut, cashew nut, almond, poppy seed, yellow melon, mango, fig, date) using HPLC/APCI-MS with a response factor approach. Average parameters and relative fatty acid concentrations are calculated with both HPLC/APCI-MS and GC/ FID.
Fats in the diet of countries in the Mediterranean basin are typically represented by olive oil, but the high consumptions of vegetables and to some extent also of fish result in appreciable intakes of n-3 fatty acids. In fact, various plant foods are relatively rich in the 18 carbon n-3 fatty acid, alpha linolenic acid, ALA, while the generally moderate consumption of fish, except for certain communities living close to the sea, contributes to the intake of the long-chain n-3. Although the amounts of fats in ALA-containing plant foods are low, the relatively high concentrations of this fatty acid and the large size of the portions consumed allow to reach appreciable doses of ALA, an n-3 fatty acid that has been shown to exert favourable effects on various relevant factors in cardiovascular protection. In addition, consumption of relatively small amounts of certain typical dry fruit components of the diet such as walnuts, provides a sizable supply of ALA that is also rather efficiently converted to the ALA derivative eicosapentaenoic acid (EPA). Additional rather typical wild food components of the diet in certain countries, i.e. snails and frogs, are also appreciable sources of ALA. It appears thus that the consumption of typical Mediterranean foods provides relevant intakes of n-3 fatty acids, especially ALA, that appears to be efficiently absorbed and also transformed at least to the long-chain derivative EPA.
The ability of vitamin E to modulate signal transduction and gene expression has been observed in numerous studies; however, the detailed molecular mechanisms involved are often not clear. The eight natural vitamin E analogues and synthetic derivatives affect signal transduction with different potency, possibly reflecting their different ability to interact with specific proteins. Vitamin E modulates the activity of several enzymes involved in signal transduction, such as protein kinase C, protein kinase B, protein tyrosine kinases, 5-, 12-, and 15-lipoxygenases, cyclooxygenase-2, phospholipase A2, protein phosphatase 2A, protein tyrosine phosphatase, and diacylglycerol kinase. Activation of some these enzymes after stimulation of cell surface receptors with growth factors or cytokines can be normalized by vitamin E. At the molecular level, the translocation of several of these enzymes to the plasma membrane is affected by vitamin E, suggesting that the modulation of protein-membrane interactions may be a common theme for vitamin E action. In this review the main effects of vitamin E on enzymes involved in signal transduction are summarized and the possible mechanisms leading to enzyme modulation evaluated. The elucidation of the molecular and cellular events affected by vitamin E could reveal novel strategies and molecular targets for developing similarly acting compounds.
Anthocyanins were the main polyphenol components in extracts of fresh and pickled red cabbage. The composition of anthocyanins in red cabbage was studied using liquid chromatography mass-spectrometry. Eleven major peaks absorbing at 520 nm were discerned, which represented 18 different anthocyanin structures. Another five minor anthocyanin components could be identified by searching at their respective m/z values but only in anthocyanin-enriched concentrates produced by sorption to solid phase extraction matrices. The predominant anthocyanins were constructed of cyanidin-3-diglucoside-5-glucoside "cores" which were non-acylated, mono-acylated or di-acylated with p-coumaric, caffeic, ferulic and sinapic acids. Pelargonidin-3-glucoside and novel forms of cyanidin-3-O-triglucoside-5-O-glucoside di-acylated with hydroxycinnamic acids were also detected in extracts of raw red cabbage, commercially pickled red cabbage and anthocyanin-enriched concentrates. The stability of the anthocyanins to simulated gastrointestinal digestion was assessed. The anthocyanins were effectively stable in the acidic gastric digestion conditions but the total recovery after simulated pancreatic digestion was around 25% compared to around 100% recovery of phenol content. As anthocyanins make up the majority of red cabbage polyphenols, this suggested that anthocyanins broke down to form new phenolic components. The recovery of the individual anthocyanins was monitored by LC-MS(n). All of the anthocyanins were reduced in content after pancreatic digestion but acylated forms were notably more stable than non-acylated forms. There was also a relationship between the type of acylated hydroxycinnamic acid and stability to pancreatic digestion.
During the last 90 years since the discovery of vitamin E, research has focused on different properties of this molecule, the focus often depending on the specific techniques and scientific knowledge present at each time. Originally discovered as a dietary factor essential for reproduction in rats, vitamin E has revealed in the meantime many more important molecular properties, such as the scavenging of reactive oxygen and nitrogen species with consequent prevention of oxidative damage associated with many diseases, or the modulation of signal transduction and gene expression in antioxidant and non-antioxidant manners. Research over the last 30 years has also resolved the biosynthesis and occurrence of vitamin E in plants, the proteins involved in the cellular uptake, tissue distribution and metabolism, and defined a congenital recessive neurological disease, ataxia with vitamin E deficiency (AVED), characterized by impaired enrichment of alpha-tocopherol in plasma as a result of mutations in the liver alpha-tocopherol transfer gene. This review is giving a brief introduction about vitamin E by following the major research directions since its discovery with a historical perspective.
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