Accelerated solvent extraction of ochratoxin a from rice samples

In this paper, accelerated solvent extraction (ASE) for the analysis of ochratoxin A (OTA) is applied for the first time. Optimization of the method is given for the extraction of OTA from rice samples. Several parameters such as type of solvent, temperature, pressure, static time, and cell size were investigated thoroughly to find the optimal extraction conditions. The optimum ASE operating conditions were methanol as extraction solvent, 1500 psi, 40 degrees C, 5 min of static time, 50% flush volume, 60 s of purge, 1 cycle, and 11 mL cell size. The total extraction time was approximately 15 min. OTA was determined by liquid chromatography coupled with a fluorescence detector and confirmed by methyl ester derivatization. The analytical performance of the method was monitored with quality control parameters. Finally, the optimized method was used to evaluate 12 rice samples, 1 of which was positive with an OTA content of 4.17 ng/g. The proposed method offers the possibility of a fast and simple process to obtain a quantitative extraction of OTA.     

Fat extraction from acid- and base-hydrolyzed food samples using accelerated solvent extraction

This paper describes a new in-cell method for pursuing accelerated solvent extraction (ASE) prior to lipid analysis from food samples. It is difficult to pursue direct ASE with acid- or base-hydrolyzed samples due to the corrosive nature of the reagents and material limitations. In this study ion exchange based materials were used to remove acid or base reagents in-cell without compromising the recovery of lipids. The performance data are presented here for the new methods for lipid extraction for a variety of food samples and compared to the Mojonnier method. NIST Standard Reference Materials (SRM-1546 and SRM-1849) were used to validate the ASE methods. Excellent fat recoveries were obtained for the ASE methods. The new methods presented here enhance the utility of ASE and eliminate labor intensive protocols.     

Disposable cartridge extraction of retinol and alpha-tocopherol from fatty samples

A new approach is proposed for liquid/solid extraction of retinol and alpha-tocopherol from samples, using a disposable kieselguhr cartridge. The substitution of the mixture methanol-ethanol-n-butanol (4 + 3 + 1) for methanol in the alkaline hydrolysis solution makes it now possible to process fatty samples. Methanol is necessary to solubilize the antioxidant ascorbic acid, and a linear chain alcohol such as n-butanol is necessary to reduce the size of soap micelles so that they can penetrate into the kieselguhr pores. In comparisons of the proposed method with conventional methods on mineral premixes and fatty feedstuffs, recovery and accuracy are at least as good by the proposed method. Advantages are increased rate of determinations and the ability to hydrolyze and extract retinol and alpha-tocopherol together from the same sample.     

Effects of different chloroform stabilizers on the extraction efficiencies of phospholipid fatty acids from soils

Chloroform is commonly used as an organic solvent to extract phospholipid fatty acids from soil samples. However, the extraction efficiency of the fatty acids depends on the particular chloroform stabilizers used. The effect of chloroform stabilizers 2-methyl-2-butene and ethanol was investigated at different steps of the extraction procedure. Only the ethanol stabilized chloroform prevented the loss of certain phospholipid fatty acids. In particular, the unsaturated fatty acids 16:1ω7c, 16:1ω6c, 16:1ω5, 17:1ω8, 18:1ω7c, 18:1ω5, the fungal biomarker 18:2ω6,9 and the saturated fatty acid 17:0 were absent when chloroform stabilized with 2-methyl-2-butene was used. In addition, the total phospholipid fatty acid concentrations were also significantly reduced when chloroform stabilized with 2-methyl-2-butene was used. Thus, the proper choice of chloroform stabilizer for the analysis of phospholipid fatty acids is very important.     

Development of a rapid method for the sequential extraction and subsequent quantification of fatty acids and sugars from avocado mesocarp tissue

Methods devised for oil extraction from avocado (Persea americana Mill.) mesocarp (e.g., Soxhlet) are usually lengthy and require operation at high temperature. Moreover, methods for extracting sugars from avocado tissue (e.g., 80% ethanol, v/v) do not allow for lipids to be easily measured from the same sample. This study describes a new simple method that enabled sequential extraction and subsequent quantification of both fatty acids and sugars from the same avocado mesocarp tissue sample. Freeze-dried mesocarp samples of avocado cv. Hass fruit of different ripening stages were extracted by homogenization with hexane and the oil extracts quantified for fatty acid composition by GC. The resulting filter residues were readily usable for sugar extraction with methanol (62.5%, v/v). For comparison, oil was also extracted using the standard Soxhlet technique and the resulting thimble residue extracted for sugars as before. An additional experiment was carried out whereby filter residues were also extracted using ethanol. Average oil yield using the Soxhlet technique was significantly (P < 0.05) higher than that obtained by homogenization with hexane, although the difference remained very slight, and fatty acid profiles of the oil extracts following both methods were very similar. Oil recovery improved with increasing ripeness of the fruit with minor differences observed in the fatty acid composition during postharvest ripening. After lipid removal, methanolic extraction was superior in recovering sucrose and perseitol as compared to 80% ethanol (v/v), whereas mannoheptulose recovery was not affected by solvent used. The method presented has the benefits of shorter extraction time, lower extraction temperature, and reduced amount of solvent and can be used for sequential extraction of fatty acids and sugars from the same sample.     

Rapid extraction and analysis of volatile fatty acids in soil

Abstract

The concentrations of volatile fatty acids (VFA) in soils are important in studies involving phytotoxicity and fermentation processes. Concentrations of acetic, propionic, and butyric acids as low as 0.21, 0.14, and 0.10 mmol kg^‐1soil in water extracts were accurately determined. The extracts were filtered through 45 μm millipore disc filters and injected directly into a gas chromatograph following addition of purified formic acid. The formic acid eliminated ghosting of peaks. The gas chromatograph was equipped with a flame ionization detector and a 60/80 Carbopack C/0.3% Carbowax 20M/0.1% H₃PO₄packed precolumn (0.15 m) and column (1.83 m). The precolumn was changed after 150 to 200 sample injections when contaminated beyond acceptable limits. There was good separation of VFA with no interfering organic volatiles in extracts of soil containing glucose, cellulose or straw incubated anaerobically for as long as 4 weeks. The advantages of the procedure are relative rapidity and simplicity as well as improved sensitivity in measuring small quantities of volatile fatty acids in soil     

A field method to store samples from temperate mountain grassland soils for analysis of phospholipid fatty acids

The storage of soil samples for PLFA analysis can lead to shifts in the microbial community composition. We show here that conserving samples in RNAlater, which is already widely used to store samples for DNA and RNA analysis, proved to be as sufficient as freezing at?-20?°C and preferable over storage at 4?°C for temperate mountain grassland soil. The total amount of extracted PLFAs was not changed by any storage treatment. Storage at 4?°C led to an alteration of seven out of thirty individual biomarkers, while freezing and storage in RNAlater caused changes in the amount of fungal biomarkers but had no effect on any other microbial group. We therefore suggest that RNAlater could be used to preserve soil samples for PLFA analysis when immediate extraction or freezing of samples is not possible, for example during sampling campaigns in remote areas or during transport and shipping.     

Comparison of solvent extraction and microwave extraction for release of dimethyl sulfide from cereals and canola

Natural levels of dimethyl sulfide (DMS) in newly harvested wheat, barley, paddy, and canola were determined by gas chromatography using a flame photometric detector in sulfur mode. The two methods involved determination of DMS in the headspace of cereal or oilseed samples (1) after extraction with microwaves and (2) after a traditional approach using 25% KBr solution. Quantitative results from each method were similar, and therefore both methods are suitable for the determination of DMS in grains and oilseeds. However, the microwave procedure has several advantages; for example, results are obtained very quickly, and only a small amount of sample is required.     

Comparison of different extraction solvent mixtures for characterization of phenolic compounds in strawberries

Eight different solvent mixtures containing acetone or methanol pure or combined with an acid (acetic, formic, hydrochloric) were tested for their efficiency for extraction of phenolic compounds from strawberries belonging to five groups of polyphenols: anthocyanins, flavonols, flavan-3-ols, hydroxycinnamic acid derivatives and conjugated forms of ellagic acid. Twenty-eight compounds from these five groups have been detected and quantified using HPLC-DAD-ESI-MS(n). The yield of each phenolic compound and group was evaluated with regard to the extraction solvent composition. Acetone containing extraction mixtures were superior to the ones containing methanol for extraction yield of total phenolic compounds, which was especially pronounced for the groups of flavan-3-ols and conjugated forms of ellagic acid. The mixture acetone/acetic acid (99:1, v/v) gave the best results for the qualitative and quantitative assay of the polyphenols present in strawberries since all 28 compounds were detected only in these extracts in quantities higher or comparable to the other extraction solvents tested.     

从沉积物中分离重金属不同提取方法的比较

Three extraction methods, ultrasonic assisted extraction (USE), microwave assisted extraction (MSE), and conventional single extraction (CSE), in conjunction with the modified three-stage BCR sequential extraction procedure (SEP) were applied to examine the contents of Cd, Cu, Cr, Ni, Pb and Zn from lake sediment samples, to know whether these techniques can reduce extraction time and improve reproducibility. The SEP and developed alternative single extraction methods were validated by the analysis of certified reference material BCR 601. By the use of optimized sonication and microwave conditions, steps 1, 2 and 3 of the BCR sequential extraction methods (excluding the hydrogen peroxide digestion in step 3, which was not performed with sonication and microwave) could be completed in 15-30 min and 60- 150 s, respectively. The recoveries of total extractable metal contents in BCR 601, obtained by three single extractions ranged from 93.3%-102%, 88.9%-104% and 81.2%-96.2% for CSE, USE and MSE, respectively. The precision of the single extraction methods was found in the range of 3.7%-9.4% for all metals (n = 6).     

溶剂萃取与生物降解法联合修复老化石油污染土壤

This study aimed to evaluate the efficacy, practicality and sustainability of a combined approach based on solvent extraction and biodegradation to remediate the soils contaminated with high levels of weathered petroleum hydrocarbons. The soils used in this study were obtained from the Shengli Oilfield in China, which had a long history of contamination with high concentrations of petroleum hydrocarbons. The contaminated soils were washed using a composite organic solvent consisting of hexane and pentane (4:1, v/v) and then bioremediated in microcosms which were bioaugmentated with Bacillus subtilis FQ06 strains and/or rhamnolipid. The optimal solvent extraction conditions were determined as extraction for 20 min at 25 °C with solvent-soil ratio of 6:1 (v/w). On this basis, total petroleum hydrocarbon was decreased from 140 000 to 14 000 mg kg-1, which was further reduced to < 4 000 mg kg-1 by subsequent bioremediation for 132 d. Sustainability assessment of this integrated technology showed its good performance for both short- and long-term effectiveness. Overall the results encouraged its application for remediating contaminated sites especially with high concentration weathered hydrocarbons.     

Lipid [corrected] classes, fatty acids, and sterols in seafood from Gilbert Bay, southern labrador

Seafood from Gilbert Bay, southern Labrador, was sampled for lipid classes, fatty acid, and sterol composition. Gilbert Bay is a proposed Marine Protected Area, and the composition of seafood from this region is interesting from both human health and ecological perspectives. Analyses included four species of bivalves and flesh and liver samples from four fish species. Lipids from a locally isolated population of northern cod (Gadus morhua) were also compared to lipids from other cod populations. Lipid classes were analyzed by Chromarod/Iatroscan TLC-FID, fatty acids by GC, and sterols by GC-MS. Three cod populations had similar levels of total lipid per wet weight (0.6%) with triacylglycerols (TAG), sterols, and phospholipids comprising on average 13, 11, and 51%, respectively, of their total lipids. Fatty fish such as capelin and herring contained on average 8.4% lipid with 86% present as TAG. Fish livers from cod and herring showed opposite trends, with cod having elevated lipid (27%) and TAG (63%) and herring containing only 3.8% lipid and 20% TAG. Shellfish averaged 0.6% lipid; however, significant lipid class differences existed among species. Fatty acid analysis showed few significant differences in cod populations with on average 57% polyunsaturated fatty acids (PUFA), 18% monounsaturated fatty acids (MUFA), and 24% saturated fatty acids (SFA). Cod livers had lower PUFA (34%) and elevated MUFA (44%) relative to flesh. Bivalves averaged 25% SFA, 18% MUFA, and 57% PUFA, whereas scallop adductor muscle had the highest PUFA levels (63%). Bivalves contained 20 different sterols with cholesterol present as the major sterol (19-39%). trans-22-Dehydrocholesterol, brassicasterol, 24-methylenecholesterol, and campesterol individually accounted for >10% in at least one species. High levels of PUFA and non-cholesterol sterols observed in Gilbert Bay seafood demonstrate their positive attributes for human nutrition.     

Quality assessment and quantitative analysis of flavonoids from tea samples of different origins by HPLC-DAD-ESI-MS

Components of green tea ( Camellia sinensis) have been of considerable interest in recent years because of their potential utility as pharmaceutical agents, particularly for their antioxidant and anticarcinogenic activity. Responding to the increasing scientific validation of numerous health benefits of tea, a comprehensive approach was adopted to carry out analysis for the quality assessment of flavonoids in tea samples of different origins. For this purpose, extraction, separation, and mass spectrometric parameters were optimized. Extraction methods evaluated include reflux extraction, a modified accelerated solvent extraction (ASE), namely, Aquasolv extraction, and microwave-assisted extraction (MAE) using different percentages of solvents. Separation was performed by a specifically developed reversed phase high-performance liquid chromatography (RP-HPLC) method using different C18 and C8 stationary phases. Optimization of extraction techniques clearly proved the performance of MAE, which delivered highest yields in a very short time. Additionally, the comparison with Aquasolv extraction provided new insights, as variations in quantified amounts of target compounds between the extracts could be explained on the basis of thermal degradation and epimerization phenomena. Especially the epimerization phenomenon for catechin/epicatechin oligomers, that is, of procyanidins P 2 and P 3, was observed for the first time. Finally, an optimized extraction and separation system was used for qualitative and quantitative investigations of compounds from different green tea samples from Ceylon (cultivated under biologically controlled conditions), Japan, India, and China as well as from one black tea sample from India.     

马铃薯生全粉中不饱和脂肪酸微波萃取工艺参数优化及应用

为了优化马铃薯生全粉不饱和脂肪酸的微波萃取工艺,该试验采用软件Design-Expert 8.05分析以及响应面法来优化马铃薯生全粉中不饱和脂肪酸微波萃取工艺,得出马铃薯生全粉中不饱和脂肪酸的萃取模型P=0.000 10.01,R2=0.939 8,并确定马铃薯生全粉中不饱和脂肪酸最佳萃取工艺:萃取温度81℃,萃取时间11 min,萃取溶剂中丙酮占比0.802 5,料液比3.25∶1,各因素对不饱和脂肪酸质量分数影响大小分别为:丙酮占比料液比萃取温度萃取时间,实测不饱和脂肪酸质量分数为1.081 mg/g和拟合方程的预测值1.084 mg/g基本一致。将该优化方案应用于热风干燥温度对马铃薯生全粉中不饱和脂肪酸含量影响的分析中,结果表明:随着干燥温度的升高,亚油酸质量分数显著增加(P0.05),总不饱和脂肪酸质量分数增加(P0.05)。优化试验为热风干燥条件对马铃薯品质影响的研究提供了理论依据。     

Accelerated solvent extraction and gas chromatography/mass spectrometry for determination of polycyclic aromatic hydrocarbons in smoked food samples.

Accelerated solvent extraction (ASE) is a new sample extraction method offering a number of advantages such as low pe -extraction cost, reduced solvent and time consumption, and simplified extraction protocols. In this study, the ASE method was applied to the extraction of polycyclic aromatic hydrocarbons (PAHs) from biological samples. For recovery studies, fish tissues and ground pork were used as sample matrices. Sample aliquots fortified with 16 PAHs were extracted by ASE, and the extracts were treated with sulfuric acid and Florisil, followed by gas chromatography-mass spectrometry analysis. The PAH recoveries by the ASE method were found to be comparable with or better than those by Soxhlet extraction. The extraction and quantitation method was then applied to the determination of PAHs in several smoked meat samples obtained from a local market. Up to 12 PAHs were found to be present at concentrations ranging from 3 to 52 ng/g wet sample.     

Ascorbic acid as a reductant for extraction of iron-bound phosphorus in soil samples: a method comparison study

Sequential extraction is commonly used to identify and quantify different forms of phosphorus (P) associated with particulate samples. Iron (Fe)-bound P is an important fraction of total particulate phosphorus because iron (Fe) is ubiquitous in natural environments. Three reductant solutions, i.e., sodium hydroxide (NaOH), dithionite, and ascorbic acid, have been used to extract solid phase reactive iron and associated phosphorus from sediments and soils. This study compares the efficiencies of three different methods in extracting Fe and Fe-bound P and evaluates the potential and limitation of each method. Based on the results of this comparative study it is recommended that the ascorbic acid reduction method is used for extraction of Fe-bound P in particulate samples, such as soil and sediment.     

Special features of humus acids extraction from soils by sodium pyrophosphate solutions of different alkalinity

The regularities of extracting humus acids from soils of different types with solutions of sodium pyrophosphate at the equilibrium pH values of 5–13 were studied. The increase in the humus acids yield from the soils with the increasing alkalinity of the solution applied is directly related to the capability of acid functional groups (carboxyl and phenol hydroxyl) for dissociation at definite pH values. The regularities of the changes in the chemical nature and degree of humification of humus acids extracted from the soils related to the pH of the solution were revealed. A sodium pyrophosphate solution (pH 10) was suggested for extracting the humus acids most active in the given soil.     

Spray-dried multilayered emulsions as a delivery method for omega-3 fatty acids into food systems

Emulsion can be produced with electrostatic layer-by-layer deposition technologies to have cationic, thick multilayer interfacial membranes that are effective at inhibiting the oxidation of omega-3 fatty acids. This study investigated the stability of spray-dried multilayer emulsion upon reconstitution into an aqueous system. The primary (lecithin) and multilayered secondary emulsions (lecithin and chitosan) were spray-dried with corn syrup solids (1-20 wt %). The lecithin-chitosan multilayer interfacial membrane remained intact on the emulsion droplets upon reconstitution into an aqueous system. Reconstituted secondary (lecithin-chitosan) emulsions were more oxidatively stable than reconstituted primary (lecithin) emulsions. A minimum of 5 wt % corn syrup solids was needed to microencapsulate the secondary emulsion droplets. Maximum oxidative stability of both the powder and the reconstituted secondary emulsions was observed in samples with 5% and 20% corn syrup solids. Addition of EDTA (25 microM) inhibited oxidation of reconstituted primary and secondary emulsions. These studies suggest that a microencapsulated multilayered emulsion system could be used as a delivery system for omega-3 fatty acids in functional foods.     

Improving the fatty acid profile of fairy shrimp, Streptocephalus dichotomus, using a lipid emulsion rich in highly unsaturated fatty acids

Fatty acids are the largest component of lipids and have become a useful tool in the determination of live feeds to a variety of cultured species. Bioencapsulation is a technique which allows high-level incorporation of desired components (i.e., fatty acids, vitamins, antibiotics, etc.) in live feeds, which in turn can be supplemented to the consumer organisms. The procedure described in the present study serves as a platform of technology for enriching the Streptocephalus dichotomus. Uptake of two enrichment diets (ALGAMAC2000 and DHA-SELCO) by adult S. dichotomus was investigated. The fatty acid profile supports the hypothesis that the enrichment diet increases the level of essential fatty acids, such as linolic, linolenic, eicosapentenoic, and docosahexaenoic acids. The average content (percent of total fatty acids detected) of the enriched organism by different highly unsaturated fatty acid (HUFA) products were as follows: ALGAMAC2000 showed 14-22% saturated fatty acid (SFA), 17-18% monounsaturated fatty acid (MUFA), 28-41% polyunsaturated fatty acid (PUFA), 23-34% n-3, and 4.9-7.5% n-6, whereas DHA-SELCO showed about 20-23% SFA, 20-26% MUFA, 38% PUFA, 28-31% n-3, and 7.5-10% n-6. Our present investigation proves that both HUFA-rich diets appear to be an appropriate enrichment diet, and further provides an additional rationale for using fairy shrimp as a maturation diet for any cultivable freshwater organism.     

Effects of vitamin E supplementation on lipid peroxidation and color retention of salted calf muscle from a diet rich in polyunsaturated fatty acids.

The color of fresh meat is one of the most important quality criteria of raw muscle foods. This red color is principally due to the presence of oxymyoglobin. The present study was undertaken to examine the effect of a diet rich in polyunsaturated fatty acids (PUFA), the addition of NaCl, and the influence of dietary supplementation with vitamin E on calf muscle oxymyoglobin oxidation (color) and lipid peroxidation. Vitamin E was added to the feed at a concentration of 4000 mg/day for 90 days before slaughter. This diet increased the alpha-tocopherol concentration in muscle membrane from 2.6-2.8 to 6.5-7.0 microg/g of fresh weight. It was found that the diet rich in PUFA and, especially, the addition of NaCl increased muscle lipid peroxidation and oxymyoglobin oxidation as indicated by the contents of thiobarbituric acid-reactive substances and substances that impaired color value readings during storage at 4 degrees C. Both undesirable reactions during storage were controlled very efficiently by the presence of a critically high concentration of alpha-tocopherol in the muscle tissues. The findings concerning the antioxidant activity of alpha-tocopherol in this study form additional evidence of its efficient protection against oxidative reactions during storage of muscle tissues and its potential to maintain a high nutritional value in them.