Rapid and direct detection of artificially aged papers employing easy ambient sonic-spray ionization mass spectrometry.

RATIONALE: The effort to make fake documents look real leads to the use of crickets and beverages to produce artificially aged papers, as land titles, based on yellowing caused by the use of these methods. An old practice in Brazil, called "cricketing", has led to the misappropriation of Brazilian land using these documents. We propose a rapid, simple, instantaneous and non-destructive method to identify artificially aged papers by easy ambient sonic-spray ionization mass spectrometry (EASI-MS) analysis. METHODS: Three typical aging procedures were used to obtain artificially aged papers using coffee, cola drink, and crickets, with the papers being analyzed by EASI-MS. Multivariate statistical analyses were performed on the data to find the sample groups and to study the most relevant ions of each ageing procedure. High-resolution MS (HRMS) was used to obtain the exact masses and attribute formulae to relevant ions present in the samples. RESULTS: The combination of EASI-MS and multivariate statistical analyses allowed us to identify the most relevant ions to classify the adulteration of documents and HRMS identified most of these relevant ions. TMS fingerprinting in combination with multivariate analysis also demonstrated that this approach can qualitatively differentiate all the examined paper samples. CONCLUSIONS: We developed a cheap, fast and easy method that can help to elucidate counterfeit documents that have been artificially aged, helping to identify chemical additives and one that can be used in forensic laboratories.

Novel natural food colourant G8000 benefits LDL- and HDL-cholesterol in humans.

The aim of this study was to investigate the phenolic composition of a natural food colourant (G8000™) as well as its effects on plasma markers after 28-day consumption by healthy individuals at a dietary dose (70 g). Parameters of total cholesterol and its fractions, triglycerides and plasma enzymes biomarkers of muscle injury were measured. Major compounds identified in G8000™ by ESI-MS showed the presence of anthocyanins, organic acids, phenolic acids as well as monosaccharides. HDL levels significantly increased from 43 ± 10.2 mg/dL to 95 ± 16.9 mg/dL. LDL levels significantly decreased from 110 ± 40.9 mg/dL to 69 ± 39 mg/dL (p < 0.001). No significant statistical differences (p > 0.05) were observed for total cholesterol, triglycerides and VLDL. After the intake, plasma enzyme CK-MB decreased from 20 ± 12.1 U/L to 10 ± 1.9 U/L while LDH levels increased from 275 ± 124.4 U/L to 317 ± 114.7 U/L (p < 0.005). No significant differences were observed for CK levels. Taken together, dietary intake of natural colourant G8000™ was able to exert beneficial effects on atherosclerosis biomarkers.

Mutamba (Guazuma ulmifolia Lam.) fruit as a novel source of dietary fibre and phenolic compounds.

This study covers the proximate and phytochemical composition of mutamba (Guazuma ulmifolia Lam.) fruit. This fruit showed high dietary fibre (36.9%) and low moisture (10.0%) contents which justify its hardness and dryness. Nevertheless, this fruit is very appreciated due to its sweet pulp (high sucrose content, 16.3%) and attractive taste. The soluble and insoluble-bound phenolic compounds from mutamba fruit were analysed by using liquid chromatography coupled to tandem mass spectrometry (LC-MS). LC-MS identified 26 compounds. Mutamba fruit was composed mainly by soluble flavonoids (1385.9 µg/g dw), namely proanthocyanidins, and aglycones and glycosylated flavonoids. Procyanidin trimer C1 (972.8 µg/g dw) followed by procyanidin dimer B2, rutin, epicatechin, and hyperoside were the main soluble phenolics, accounting 1435.5 µg/g dw. Conversely, the main cell wall bound phenolics (228.8 µg/g dw) were catechin, followed by protocatechuic acid, epicatechin, and gallic acid. In conclusion, mutamba fruit may be a novel source of dietary fibre and bioactive phenolic compounds.

LC-MS/MS screening and identification of bioactive compounds in leaves, pulp and seed from Eugenia calycina Cambess.

The Eugenia calycina Cambess, also known as pitanga-do-cerrado, is an unexplored Brazilian fruit used by native people for the treatment of diabetes. The aim of this study was to identify the phenolic compounds from the leaves, pulp and seed of Eugenia calycina by using LC-MS-based targeted and untargeted analysis. The LC-MS-based targeted quantitative analysis showed a high phenolic content in all plant parts in which the ellagic acid was the main phenolic compound with values of 8244.53 µg/g dw (leaves), 5054.43 µg/g dw (pulp) and 715.42 µg/g dw (seed). The leaves, pulp and seed showed a high total phenolic content of 20371.96, 7139.70 and 2204.75 µg/g dw, respectively. In addition, the LC-MS-based targeted analysis showed ellagic acid, myricitrin and epicatechin gallate as the main phenolic compounds in the Eugenia calycina. The LC-MS-based untargeted analysis showed the phytochemical profile of the leaves, pulp and seed in which 153 phytochemicals from different chemical classes were annotated, including organic acids, phenolic acids, flavonoids, and other compounds. The Eugenia calycina has high potential as a plant-based food due to its phytochemical profile and high phenolic content.

[Different lipid extraction methods on fatty acids composition in cow milk]. / Avaliação de diferentes métodos de extração lipídica sobre a composição de ácidos graxos poliinsaturados em leite de vaca.

Different lipid extraction methods on fatty acids composition in cow milk. Comparative studies among 4 (four) different methods of total lipids extraction were carried out to evaluate the lipid extraction efficiency and fatty acids contents in cow milk. Total lipids extraction methods were Bligh e Dyer (BD), Folch et al. (FLS), Roese-Gottlieb (RG) and Gerber (GB). There were non-significant (p < 0.05) difference, in total lipids content among the extraction methods. The smallest concentrations of omega-3 (n-3) fatty acids and polyunsaturated fatty acids (PUFA) were observed on method GE, possibly due degradation of PUFA immersed in sulfuric acid used during analysis of total lipids. The highest concentrations of n-3 PUFA were observed by BD method, especially to omega-3/omega-6 ratio and alpha-linolenic acid (LNA, 18:3n-3), eicosapentaenoic (EPA, 20:5n-3) and docosahexaenoic (DHA, 22:6n-3), significant differences were observed among the methods. The results demonstrate that the different extractions influenced decisively on quantitative fatty acids composition and evaluations indicated the methods BD as better and GE as the worst to polyunsaturated fatty acids determination.

Characterization of the lipid profile from coconut (Cocos nucifera L.) oil of different varieties by electrospray ionization mass spectrometry associated with principal component analysis and independent component analysis.

Coconut oil (CO) from fifteen different varieties of coconuts (Cocos nucifera L.) and one CO processed on an industrial scale were analyzed by electrospray ionization mass spectrometry (ESI-MS) and the data processed using the chemometric tools principal component analysis and independent component analysis. ESI-MS fingerprinting of lipid compounds showed predominance of diacylglycerols and triacylglycerols, as confirmed by high-resolution MS measurements. Chemometric processing of the ESI-MS data differentiated the coconut oil samples, showing that different coconut varieties/cultivars produce oils with distinguishable abundances of lipidic compounds. Thus ESI-MS analysis followed by data treatment using chemometric tools offers a tool able to classify the industrial coconut oils in a fast, simple and effective way, as well as serving as a potential method to identify the coconut varieties by the CO origin, and the occurrence of any adulteration. The procedure may also be applied for quality control of the industrial processes.

Amazon climatic factors driving terpene composition of Iryanthera polyneura Ducke in terra-firme forest: A statistical approach.

Iryanthera polyneura (Myristicaceae) is popularly known as cumala-colorada, and can be found in the Amazon rain forest. The present study aimed the evaluation of the chemical composition of the essential oils (EOs) obtained from the leaves of I. polyneura throughout a two-year period in order to correlate chemical findings with seasonality and climatic variation. Leaves from I. polyneura were collected 15 times from three different individuals, identified as 22EO, 80EO and 530EO, between the years of 2009 and 2011. The EOs were obtained and tested by gas-chromatography-mass spectrometry techniques. ANOVA and multivariate analyses were used to assess the relationship between the percentage of terpenes and seasonal/climatic variations. Fifty-nine compounds were detected in the EOs, of which 44 were identified (74.5%). The main components of the EOs were spathulenol (6.42 ± 1.02%), α-cadinol (5.82 ± 0.40%) and τ-muurolol (5.24 ± 0.03%). Higher levels of spathulenol were observed in 22EO during rainy season, while τ-muurolol occurred in high amounts during the dry season, as did α-cadinol in 22EO and 80EO. Correspondence analysis revealed a distinction between two groups of EOs based on seasonality, whereas a canonic correspondence analysis and ANOVA determined how the major compounds were related to both seasonality and climatic factors. Non-metric multidimensional scaling in association with an analysis of similarities showed that the abundance and composition of terpenes in the samples varied moderately among the three Iryanthera individual plants. Present findings have shown that there is variation in the occurrence of the major compounds spathulenol, τ-muurolol and α-cadinol produced by I. polyneura and that the pattern of variation is related to season and climatic changes.

Carbohydrates, volatile and phenolic compounds composition, and antioxidant activity of calabura (Muntingia calabura L.) fruit.

Soluble carbohydrates, volatile and phenolic compounds from calabura fruit as well as its antioxidant activity were assessed. The low amount of fermentable oligo-, di-, and monosaccharides and polyols (FODMAPs) and similar amount of glucose and fructose allow us to classify the calabura berry as low-FODMAPs. The terpenes ß-Farnesene and dendrolasin identified by SPME-GC-MS were the major volatile components. UHPLC-MS/MS analysis revelled gallic acid (5325 µg/g dw) and cyanidin-3-O-glucoside (171 µg/g dw) as the main phenolic compounds, followed by gentisic acid, gallocatechin, caffeic acid and protocatechuic acid. In addition, gallic acid was found mainly in esterified (2883 µg/g dw) and insoluble-bound (2272 µg/g dw) forms. Free and glycosylated forms showed however the highest antioxidant activity due to occurrence of flavonoids (0.28-27 µg/g dw) in these fractions, such as catechin, gallocatechin, epigallocatechin, naringenin, and quercetin. These findings clearly suggest that calabura is a berry with low energy value and attractive colour and flavour that may contribute to the intake of several bioactive compounds with antioxidant activity. Furthermore, this berry have great potential for use in the food industry and as functional food.

Determination of free, esterified, glycosylated and insoluble-bound phenolics composition in the edible part of araticum fruit (Annona crassiflora Mart.) and its by-products by HPLC-ESI-MS/MS.

Phenolics present in the free, esterified, glycosylated and insoluble-bound forms of araticum pulp, peel and seed were for the first time characterized and quantified using HPLC-ESI-MS/MS. Levels of total phenolics, flavonoids, condensed tannins and antioxidant activities from araticum fruit followed the order peel > pulp > seed. Overall, insoluble-bound and esterified phenolics were the dominant forms of phenolics from araticum fruit parts and the highest contributors to their antioxidant activities. Extracts were found to contain contrasting levels of phenolics that were specific to each fruit part. From 10 phenolics quantified in araticum fruit, catechin and epicatechin were the major ones from pulp and peel, whereas seed displayed caffeic acid, catechin and epicatechin as its main phenolics. Araticum fruit was found to provide a good source of phenolics, and the full exploitation of this fruit may find applications in the food, cosmetic and pharmaceutical industries.

Effect of flaxseed oil in diet on fatty acid composition in the liver of Nile tilapia (Oreochromis niloticus).

This study analyzed the effects of different concentrations of flaxseed oil (FO) on the proximate composition and the contents of alpha-linolenic acid (LNA, 18:3n-3), eicosapentaenoic (EPA, 20:5n-3), and docosahexaenoic (DHA, 22:6n-3) fatty acids in the liver of cultured Nile tilapia (Oreochromis niloticus). During the five-month culture period, tilapias were given diets with incremental concentrations of FO (0.00%; 1.25%; 2.50%; 3.75%, and 5.00%) as a replacement of sunflower oil (control). There was no significant difference in moisture and ash content in the liver between treatments. Protein values ranged from 12.1% (treatment II) to 13.9% (treatment V) and total lipids ranged from 5.6% (treatment V) to 7.2% (treatment II). There was no significant difference between most treatments. Fatty acid methyl esters (FAMEs) were quantitatively analyzed by capillary gas chromatography against a C(23:0), internal standard. Variations in concentrations (in mg g(-1) of total lipids) of fatty acids between treatment I and treatment V ranged from 4.2 to 51.2 (LNA), from 0.2 to 2.3 (EPA), and from 10.6 to 56.2 (DHA), respectively. This experiment demonstrated that increasing amounts of LNA in feed may markedly increase the amounts of LNA, EPA, and DHA in the liver of Nile tilapia.

EASI-IMS an expedite and secure technique to screen for 25I-NBOH in blotter papers.

The increasing number of new psychoactive substances (NPS) and their quick worldwide spreading, often only slightly modified in the form of new derivatives and analogues, have brought the need for fast, wide-ranging, and unequivocal identification methods in clinical and forensic investigations. Because it usually provides secure results, gas chromatography coupled to mass spectrometry (GC-MS) has been routinely employed as the standard technique for the detection of NPS in blotter papers. For 25I-NBOH (N-(2-hydroxybenzyl)-2-(4-iodo-2,5-dimethoxyphenyl)ethan-1-aminium), however, GC-MS analysis of an blotter paper extract leads to incorrect results. In this work, we investigated whether easy ambient sonic-spray mass spectrometry imaging (EASI-IMS), and ambient ionization MS method can be applied directly to the surface of the sample requiring therefore no extraction or sample preparations, would serve as an efficient, sensitive, and secure alternative for 25I-NBOH screening.

A single administration of fish oil inhibits the acute inflammatory response in rats.

OBJECTIVE: To investigate the antiinflammatory effects of a single administration of fish oil (FO) on the acute inflammatory response. METHODS: The paw edema and pleurisy models were used to evaluate the effects of FO dissolved in olive oil (FOP) orally administered in a single dose in rats. Nitric oxide (NO) concentrations in the pleural exudate were performed according to the Griess method and the cytokine concentrations were determined by Luminex bead-based multiplex assay. RESULTS: FOP treatment (30 and 300 mg/kg) significantly reduced paw edema. FOP treatment at 18.75, 37.5, 75.0, 150.0, and 300 mg/kg decreased both the volume of pleural exudate and cellular migration into the pleural cavity and each of these doses presented the same effectiveness. Treatment with FOP (300 mg/kg) reduced NO, TNF-α, IL-1ß, and IL-6 concentrations in the pleural exudate. CONCLUSIONS: The present data provide evidence that FO has inhibitory effects on the acute inflammatory response when administered in a single dose in rats. This effect might be attributable to a direct inhibitory effect of FO on the production or release of inflammatory mediators that are involved in the pathological processes evaluated herein.

Forensic Application of X-ray Fluorescence Spectroscopy for the Discrimination of Authentic and Counterfeit Revenue Stamps.

Energy-dispersive X-ray fluorescence (ED-XRF) spectroscopy with data treatment via chemometric tools was explored as an analytical protocol to discriminate between authentic and counterfeit revenue stamps. Untreated samples were directly analyzed, and the discrimination was based on the characterization of constituent elements present in the inks and paper. Authentic samples and samples that were suspected of being counterfeit were analyzed at three different areas on their surfaces: the ink-printed area, the non-printed area, and the holographic area. Principal component analysis (PCA) was applied to the data to discriminate between authentic and counterfeit revenue stamps. Major differences in the elemental composition were noted (according to chemometrics and t-test, p < 0.05), and ED-XRF spectroscopy plus PCA protocol is proposed for use by non-specialist operators to screen for counterfeit stamps.

Purple carrot extract protects against cadmium intoxication in multiple organs of rats: Genotoxicity, oxidative stress and tissue morphology analyses.

The aim of this study was to investigate if purple carrot extract is able to protect against the noxious activities induced by cadmium exposure in multiple organs of rats. For this purpose, histopathological analysis, genotoxicity and oxidative status were investigated in this setting. A total of twenty Wistar rats weighing 250g on the average, and 8 weeks age were distributed into four groups (n=5), as follows: Control group (non-treated group, CTRL); Cadmium group (Cd) and Purple carrot extract groups at 400mg/L or 800mg/L. Histopathological analysis revealed that liver from animals treated with purple carrot extract improved tissue degeneration induced by cadmium intoxication. Genetic damage was reduced in blood and hepatocytes as depicted by comet and micronucleus assays in animals treated with purple carrot extract. SOD-CuZn and cytocrome C gene expression increased in groups treated with purple carrot extract. Purple carrot extract also reduced the 8OHdG levels in liver cells when compared to cadmium group. Taken together, our results demonstrate that purple carrot extract is able to protect against cadmium intoxication by means of reducing tissue regeneration, genotoxicity and oxidative stress in multiple organs of Wistar rats.

Subcritical extraction of flaxseed oil with n-propane: Composition and purity.

Flaxseed (Linum usitatissimum L.) oil was obtained via subcritical n-propane fluid extraction (SubFE) under different temperatures and pressures with an average yield of 28% and its composition, purity and oxidative stability were compared to oils obtained via conventional solvent extraction methods (SEMs). When the oxidative stability was measured by differential scanning calorimetry, the oil was found to be up to 5 times more resistant to lipid oxidation as compared to the SEM oils. Direct infusion electrospray ionization mass spectrometry (ESI-MS) analysis showed characteristic and similar TAG profiles for SubFE and SEMs oils but higher purity for the SubFE oil. The flaxseed oil content of ß-tocopherol, campesterol, stigmasterol and sitosterol were quantified via GC-MS. SubFE showed to be a promising alternative to conventional SEM since SubFE provides an oil with higher purity and higher oxidation stability and with comparable levels of biologically active components.

Characterization of ANFO explosive by high accuracy ESI(±)-FTMS with forensic identification on real samples by EASI(-)-MS.

Ammonium nitrate fuel oil (ANFO) is an explosive used in many civil applications. In Brazil, ANFO has unfortunately also been used in criminal attacks, mainly in automated teller machine (ATM) explosions. In this paper, we describe a detailed characterization of the ANFO composition and its two main constituents (diesel and a nitrate explosive) using high resolution and accuracy mass spectrometry performed on an FT-ICR-mass spectrometer with electrospray ionization (ESI(±)-FTMS) in both the positive and negative ion modes. Via ESI(-)-MS, an ion marker for ANFO was characterized. Using a direct and simple ambient desorption/ionization technique, i.e., easy ambient sonic-spray ionization mass spectrometry (EASI-MS), in a simpler, lower accuracy but robust single quadrupole mass spectrometer, the ANFO ion marker was directly detected from the surface of banknotes collected from ATM explosion theft.

Composição e estabilidade lipídica da farinha de espinhaço de tilapia / Composition and lipid stability of tilapia fishbone flour

Espinhaços de tilápias (Oreochromis niloticus) são partes do peixe de composição desconhecida. A composição lipídica dos espinhaços não é citada na literatura, bem como a estabilidade da farinha do espinhaço durante o armazenamento. Nesse sentido, realizou se estudo de processamento dos espinhaços envolvendo etapas de cocção, trituração, secagem, peneiramento e armazenamento da farinha. A farinha ficou armazenada sob refrigeração por um período de 90 dias, sendo sua qualidade monitorada por meio da composição em ácidos graxos, índice de acidez e análises microbiológicas. Os resultados da composição centesimal foram de 14,2 por cento (umidade), 40,8 por cento (proteína), 18,3 por cento (resíduo mineral fixo) e 25,3 por cento de lipídios totais. Nos lipídios totais foi identificado um total de 24 ácidos graxos, com predominância dos ácidos graxos (porcentagem média) de 27.4 por cento (ácido palmítico, 16:0), 35,15 por cento (ácido oléico, 18:1n-9) e 11,82 por cento (ácido linoléico, 18:2n-6) e, em menor proporção: 0,88 por cento (ácido alfa-linolênico, 18:3n-3), 0,08 por cento (ácido eicosapentaenóico, 20:5n-3) e 0,59 (ácido docosahexaenóico, 22:6n-3). Durante os 90 dias de armazenamento, foram observadas algumas alterações no índice de acidez e composição de alguns ácidos graxos, no entanto, para 60 dias de armazenamento, não foram observadas alterações na composição de nenhum ácido graxo, do índice de acidez e nas análises microbiológicas.

The composition of the tilapia (Oreochromis niloticus) fishbone is unknown. Lipid composition fishbone is not cited in the literature, and neither is the stability of the flour of the fishbone during storage. We studied the processing of fishbone cooking, grinding, drying, sieving and the storage of the flour. The flour was stored in a refrigerator for a period of 90 days, and its quality was monitored through fatty acid composition, acid index and microbiology control. The results of the proximate composition were of 14.2 percent (moisture), 40.8 percent (protein), 18.3 percent (ash), and 25.3 percent total lipids. In the total lipids identified 24 fatty acids were identified, with predominance of the fatty acids (medium percentage) of 27.4 percent (palmitic acid, 16:0), 35.15 percent (oleic acmid, 18:1n-9) and 11.82 percent (linoleic acid , 18:2n-6) and, in smaller proportion: 0.88 percent (alpha-linolenic acid, 18:3n-3), 0.08 percent (eicosapentaenoic acid, 20:5n-3) and 0.59 (docosahexaenoic acid, 22:6n-3). During the 90 days of storage some alterations were observed in the acid index and composition of some fatty acids, however, for 60 days of storage no alterations were observed in the fatty acids composition, acid index, and microbiology control.

Evaluation of lipid extraction and fatty acid composition of human plasma

AIM: The objective of this study was to compare the efficiency of lipid extraction and to evaluate the fatty-acid composition in total lipids from human plasma, using a new technique and the established Folch, Lees and Stanley (FLS), Bligh and Dyer (BD), Rose-Gottlieb (RG), and Gerber (GM) methods. METHOD: A new technique, the alternative method, to extract total lipids using a microwave was proposed and evaluated. RESULTS: The total lipids extracted from human plasma varied between 0.19 percent and 0.41 percent; the highest total lipid extracted were obtained by the Folch, Lees and Stanley (0.41 percent), alternative method (0.37 percent) and Rose-Gottlieb (0.36 percent) methods. The Gerber method was ineffective to extract total lipids from human plasma. A total of 24 fatty-acid species were quantified by gas chromatography. Of the methods studied, the highest concentrations were found using the Folch, Lees and Stanley method (p < 0.05). CONCLUSION: The alternative method is a fast lipid-extraction technique that can be used for the identification of human plasma fatty acids, but it is not suitable for their measurement.

OBJETIVO: O objetivo desse estudo foi comparar a eficiência da extração lipídica e avaliar a composição em ácidos graxos nos lipídios totais (LT) no plasma humano usando uma nova técnica e os métodos já conhecidos: Folch, Lees e Stanley (FLS), Bligh e Dyer (BD), Rose-Gottlieb (RG) e Gerber (MG). MÉTODO: A nova técnica para extração de lipídios totais utiza o micro-ondas, método Alternativo (MA). RESULTADOS: Os lipídios totais (LT) extraídos do plasma variaram de 0,19 por cento a 0,41 por cento, os maiores teores foram obtidos por FLS (0,41 por cento), MA (0,37 por cento) e RG (0,36 por cento). O MG foi ineficaz na extração dos lipídios totais do plasma. Um total de 24 espécies de ácidos graxos foi quantificado no plasma por cromatografia em fase gasosa. Entre os métodos estudados, as maiores concentrações de ácidos graxos foram obtidas usando-se o método de FLS (p< 0,05). CONCLUSÃO: O método Alternativo foi considerado uma técnica rápida de extração lipídica, a qual poderá ser utilizada somente na identificação de ácidos graxos em plasma humano, mas não adequado para a quantificação dos mesmos.

Avaliação de diferentes métodos de extração lipídica sobre a composição de ácidos graxos poliinsaturados em leite de vaca / Different lipid extraction methods on fatty acids composition in cow milk

Avaliação de diferentes métodos de extração lipídica sobre a composição de ácidos graxos poliinsaturados em leite de vaca. Estudos comparativos entre 4 (quatro) diferentes métodos de extração de lipídios totais foram avaliados em relação à eficiência de extração lipídica e as implicações sobre a composição de ácidos graxos no leite de vaca. As extrações de lipídios totais foram realizadas de acordo com métodos convencionalmente utilizados no mundo, essas metodologias incluem os métodos de: Bligh e Dyer (BD), Folch et al. (FLS), Roese-Goottlieb (RG) e Gerber (GE). Os resultados mostram que não houve diferença significativa (p<0,05), no teor de lipídios totais entre os métodos de extração. As menores concentrações de ácidos graxos ômega-6 e ácidos graxos poliinsaturados foram observadas no método GE, possivelmente devido à degradação pelo ácido sulfúrico, o qual foi utilizado na metodologia. As maiores concentrações dos ácidos graxos poliinsaturados da série ômega-3 (n-3) foi observada no método BD, especialmente para a razão ômega-3/ômega-6 e os ácidos alfa-linolênico (LNA, 18:3n-3), eicosapentaenóico (EPA, 20:5n-3) e docosahexaenóico (DHA, 22:6n-3), com diferenças significativas das demais metodologias. Os resultados das diferentes metodologias de extração influenciaram decisivamente nos resultados da composição quantitativa de ácidos graxos e, as avaliações indicaram o método BD como o melhor e a o método de GE como a pior na determinação quantitativas de ácidos graxos poliinsaturados em leite de vaca.

Comparative studies among 4 (four) different methods of total lipids extraction were carried out to evaluate the lipid extraction efficiency and fatty acids contents in cow milk. Total lipids extraction methods were Bligh e Dyer (BD), Folch et al. (FLS), Roese-Gottlieb (RG) and Gerber (GB). There were non-significant (p<0.05) difference, in total lipids content among the extraction methods. The smallest concentrations of omega-3 (n-3) fatty acids and polyunsaturated fatty acids (PUFA) were observed on method GE, possibly due degradation of PUFA immersed in sulfuric acid used during analysis of total lipids. The highest concentrations of n-3 PUFA were observed by BD method, especially to omega-3/omega-6 ratio and alpha-linolenic acid (LNA, 18:3n-3), eicosapentaenoic (EPA, 20:5n-3) and docosahexaenoic (DHA, 22:6n-3), significant differences were observed among the methods. The results demonstrate that the different extractions influenced decisively on quantitative fatty acids composition and evaluations indicated the methods BD as better and GE as the worst to polyunsaturated fatty acids determination.