Comparison of organic and deep eutectic solvents based dispersive liquid-liquid microextraction for the analysis of phytosterols in cow milk combined with high-performance liquid chromatography-ultraviolet detector.
TL;DR: In this article, a dispersive liquid-liquid microextraction approach has been developed for extraction of four phytosterols (stigmasterol, β-sitosterol, campesterol, and brassicasterol) from cow milk samples using organic and deep eutectic solvents and the results were critically compared.
Abstract: In the present work, a dispersive liquid-liquid microextraction approach has been developed for extraction of four phytosterols (stigmasterol, β-sitosterol, campesterol, and brassicasterol) from cow milk samples using organic and deep eutectic solvents and the results were critically compared. The extracted analytes were determined using high performance liquid chromatography. In the developed method, carbon tetrachloride and choline chloride:p-chlorophenol deep eutectic solvent were selected to use as the best extraction solvent. Effective parameters and validation data were studied for both methods, independently. Under optimum conditions, limits of detection and quantification were within the ranges of 0.3-0.9 and 1.0-3.0 ng/mL for organic solvent based dispersive liquid-liquid microextraction and 0.09-0.32 and 0.3-1.0 ng/mL for deep eutectic solvent based dispersive liquid-liquid microextraction, respectively. Good coefficient of determinations and relative standard deviations obtained for the methods were ≥0.994 and ≤7.6%, respectively. The introduced method was performed on different milk samples for the determination of target analytes using both solvents and the results were analyzed statistically by the t-test.
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TL;DR: In this article , a review is devoted to the analysis of bioactive compounds in foods using different microextraction approaches reported in the literature since 2015, which represents an opportunity to mitigate the environmental impact of organic solvents usage, as well as lab equipment.
Abstract: For a long time, the importance of sample preparation and extraction in the analytical performance of the most diverse methodologies have been neglected. Cumbersome techniques, involving high sample and solvent volumes have been gradually miniaturized from solid-phase and liquid-liquid extractions formats and microextractions approaches are becoming the standard in different fields of research. In this context, this review is devoted to the analysis of bioactive compounds in foods using different microextraction approaches reported in the literature since 2015. But microextraction also represents an opportunity to mitigate the environmental impact of organic solvents usage, as well as lab equipment. For this reason, in the recent literature, phenolics and alkaloids extraction from fruits, medicinal herbs, juices, and coffee using different miniaturized formats of solid-phase extraction and liquid-liquid microextraction are the most popular applications. However, more ambitious analytical limits are continuously being reported and emergent sorbents based on carbon nanotubes and magnetic nanoparticles will certainly contribute to this trend. Additionally, ionic liquids and deep eutectic solvents constitute already the most recent forefront of innovation, substituting organic solvents and further improving the current microextraction approaches.
9 citations
TL;DR: There are three liquid phase microextraction (LPME) configurations, including single drop micro-extraction, hollow-fibre LPME, and dispersive liquid-liquid micro extraction as mentioned in this paper .
7 citations
TL;DR: The proposed method could be successfully applied to the analysis of four types of sulfonylurea herbicides in soil samples and a good linearity was observed for each herbicide.
Abstract: In this study, switchable hydrophilic solvent-based dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography was developed for the determination of four sulfonylurea herbicides in soils. For the first time, the sample pretreatment was achieved due to the similar acid-base status of sulfonylurea herbicides and switchable hydrophilic solvent. In the extraction step, sulfonylurea herbicides were extracted as anions and transferred to an alkaline solution with switchable hydrophilic solvent anions. In the concentration step, two types of anions were transformed to their molecular state after the aqueous solution was acidfied. In addition, the dispersion and microextraction process were completed efficiently with the simultaneous formation of analytes and extractant. The factors affecting the extraction performance were optimized. Under the optimized conditions, a good linearity was observed for each herbicide with correlation coefficients ranging from 0.9952 to 0.9978. The limits of detection were in the range of 0.1-0.2 μg g-1 . Moreover, the relative recoveries of the sulfonylurea herbicides at spiking levels of 0.5, 1, 1.5 μg g-1 in soil samples were between 75% and 111% (relative standard deviations: 0.4% to 11.4%). Therefore, the proposed method in this study could be successfully applied to the analysis of four types of sulfonylurea herbicides in soil samples. This article is protected by copyright. All rights reserved.
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TL;DR: A comprehensive overview of the recently developed sample preparation methods and analytical techniques applied to determine synthetic antioxidants in edible oils from 2010 to present, with emphasis on the sample preparation method combined with separation-based analytical techniques such as CE and LC with various detectors is provided in this article .
Abstract: Synthetic antioxidants play a critical role in the storage and process of edible oil due to that they can retard lipid oxidation, maintain the quality of oils, and prolong the shelf life. However, a series of studies have proved the potential risks of synthetic antioxidants for human health when consumed in excess, and many countries have established the permitted amounts of synthetic antioxidants in oils. Thus, the accurate quantification of synthetic antioxidants in edible oils is necessary, and there have developed various analytical methods involved in chromatographical, electrochemical, and spectroscopic methods. Owing to the complex matrix and the incompatibility between the oil sample and the detection instrument, sample preparation is usually adopted prior to the instrument detection to improve the detection effectiveness. The current review aims to provide a comprehensive overview of the recently developed sample preparation methods and analytical techniques applied to determine synthetic antioxidants in edible oils from 2010 to present, with emphasis on the sample preparation methods combined with separation-based analytical techniques such CE and LC with various detectors. The advantages and limitations of some typical analytical methods are discussed and some insights in the future perspectives are also provided in this review. This article is protected by copyright. All rights reserved.
4 citations
TL;DR: In this article , the use of deep eutectic solvents (DESs) in liquid-liquid (micro) extraction (LLME) procedures is discussed, and the applications of DESs for the determination of organic and inorganic analytes in various matrices.
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References
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TL;DR: Phytosterols and phytostanols have received much attention in the last five years because of their cholesterol-lowering properties and the popularity of these products has caused the medical and biochemical community to focus much attention on phytosterol research activity.
1,014 citations
TL;DR: Since the morbidity and mortality from cardiovascular disease have been dramatically reduced using cholesterol-lowering drugs (statins), the interest in plant sterols lies in their potential to act as a natural preventive dietary product.
Abstract: Plant sterols are an essential component of the membranes of all eukaryotic organisms. They are either synthesised de novo or taken up from the environment. Their function appears to be to control membrane fluidity and permeability, although some plant sterols have a specific function in signal transduction. The phytosterols are products of the isoprenoid pathway. The dedicated pathway to sterol synthesis in photosynthetic plants occurs at the squalene stage through the activity of squalene synthetase. Although the activity of 3-hydroxymethyl-3-glutaryl coenzyme A (HGMR) is rate-limiting in the synthesis of cholesterol, this does not appear to be the case with the plant sterols. Up-regulation of HGMR appears to increase the biosynthesis of cycloartenol but not the Δ5-sterols. A decline in sterol synthesis is associated with a suppression of squalene synthetase activity, which is probably a critical point in controlling carbon flow and end-product formation. The major post-squalene biosynthetic pathway is regulated by critical rate-limiting steps such as the methylation of cycloartenol into cycloeucalenol. Little is known about the factors controlling the biosynthesis of the end-point sterol esters or stanols. The commonly consumed plant sterols are sitosterol, stigmasterol and campesterol which are predominantly supplied by vegetable oils. The oils are a rich source of the steryl esters. Less important sources of sterols are cereals, nuts and vegetables. The nutritional interest derives from the fact that the sterols have a similar structure to cholesterol, and have the capacity to lower plasma cholesterol and LDL cholesterol. Since the morbidity and mortality from cardiovascular disease have been dramatically reduced using cholesterol-lowering drugs (statins), the interest in plant sterols lies in their potential to act as a natural preventive dietary product. Stanols (saturated at C-5) occur in low amounts in the diet and are equally effective in lowering plasma cholesterol and do not cause an increase in plasma levels, unlike the sterols which can be detected in plasma.
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917 citations
TL;DR: An extraction and derivatization protocol, developed using experimental design theory, for analyzing the human blood plasma metabolome by GC/MS, suggests that the method could be usefully integrated into metabolomic studies for various purposes, e.g., for identifying biological markers related to diseases.
Abstract: Analysis of the entire set of low molecular weight compounds (LMC), the metabolome, could provide deeper insights into mechanisms of disease and novel markers for diagnosis. In the investigation, w ...
478 citations
TL;DR: Phytosterol concentrations were greater than reported in existing food composition databases, probably due to the inclusion of steryl glycosides, which represent a significant portion of total sterols in nuts and seeds.
Abstract: Phytosterols were quantified in nuts and seeds commonly consumed in the United States. Total lipid extracts were subjected to acid hydrolysis and then alkaline saponfication, and free sterols were analyzed as trimethylsilyl derivatives by capillary GC-FID and GC-MS. Δ5-Avenasterol was quantified after alkaline saponification plus direct analysis of the glucoside. Sesame seed and wheat germ had the highest total phytosterol content (400−413 mg/100 g) and Brazil nuts the lowest (95 mg/100 g). Of the products typically consumed as snack foods, pistachio and sunflower kernel were richest in phytosterols (270−289 mg/100 g). β-Sitosterol, Δ5-avenasterol, and campesterol were predominant. Campestanol ranged from 1.0 to 12.7 mg/100 g. Only 13 mg/100 g β-sitosterol was found in pumpkin seed kernel, although total sterol content was high (265 mg/100 g). Phytosterol concentrations were greater than reported in existing food composition databases, probably due to the inclusion of steryl glycosides, which represent a ...
390 citations
TL;DR: Using lipid analysis by mass spectrometry and a genetic approach on mutants in sterol metabolism, it is shown that cells adjust their membrane composition in response to mutant sterol structures preferentially by changing their sphingolipid composition.
Abstract: Sterols and sphingolipids are limited to eukaryotic cells, and their interaction has been proposed to favor formation of lipid microdomains. Although there is abundant biophysical evidence demonstrating their interaction in simple systems, convincing evidence is lacking to show that they function together in cells. Using lipid analysis by mass spectrometry and a genetic approach on mutants in sterol metabolism, we show that cells adjust their membrane composition in response to mutant sterol structures preferentially by changing their sphingolipid composition. Systematic combination of mutations in sterol biosynthesis with mutants in sphingolipid hydroxylation and head group turnover give a large number of synthetic and suppression phenotypes. Our unbiased approach provides compelling evidence that sterols and sphingolipids function together in cells. We were not able to correlate any cellular phenotype we measured with plasma membrane fluidity as measured using fluorescence anisotropy. This questions whether the increase in liquid order phases that can be induced by sterol–sphingolipid interactions plays an important role in cells. Our data revealing that cells have a mechanism to sense the quality of their membrane sterol composition has led us to suggest that proteins might recognize sterol–sphingolipid complexes and to hypothesize the coevolution of sterols and sphingolipids.
194 citations