Optimization Of Solvent Extraction Research Articles

Extraction, rapid preparation and neuroprotective effect of texasin, a main active constituent from Caragana jubata (Pall.) Poir.

Searching for new anti-ischemic stroke (anti-IS) drugs has always been a hot topic in the pharmaceutical industry. Natural products are an important source of discovering anti-IS drugs. The aim of the present study is to extract, rapidly prepare and explore the neuroprotective effect of texasin, a main active constituent from Caragana jubata (Pall.) Poir., which is a kind of Tibetan medicine with a clear anti-IS effect. The results showed that 95% ethanol was the optimal extraction solvent. A three-step rapid preparation method for texasin was successfully established, with a purity of 99.2%. Texasin at the concentration of 25–100 µM had no effect on the viability of normal cultured PC12 cells; 12.5 and 25 µM texasin could enhance the viability of PC12 cells damaged by oxygen and glucose deprivation/reoxygenation (OGD/R), and their effects are comparable to the positive drug edaravone at the concentration of 50 µM. Compared with the normal group, the expression of Bcl-2 protein in OGD/R-injured PC12 cells was downregulated (p < 0.01), and that of PERK, eIF2α, ATF4, CHOP, Bax and Cleaved caspase-3 proteins were upregulated (p < 0.01, p < 0.001). Compared with the OGD/R group, 25 µM texasin could upregulate the expression of Bcl-2 protein (p < 0.01), and downregulate that of PERK, eIF2α, ATF4, CHOP, Bax and Cleaved caspase-3 proteins (p < 0.01, p < 0.001). The 7-OH and 1-O of texasin formed H-bonds with residues Cys891 of the hinge β-strand of PERK, which is crucial for kinase inhibitors. The above results suggest that the method established in the present study achieved rapid preparation of high-purity texasin. Texasin might inhibit neuronal apoptosis via the regulation of endoplasmic reticulum stress PERK/eIF2α/ATF4/CHOP signalling pathway to exert a protective effect on OGD/R-injured PC12 cells. Aiding by molecular docking, texasin was assumed to be a potential PERK inhibitor.

Extraction, Isolation and Identification of Luteolin Flavonoid from Vitex pseudonegundo leaves

Objective: Using HPLC as a quantitative estimate technique, the optimal extraction solvent for luteolin from Vitex pseudo-negundo was identified. Methods: leaves V. pseudonegundo were gathered, washed, and dried. employeing methanol and ethanol as the extraction solvents (both with varied strengths), as well as the extraction techniques of maceration, reflux, and Soxhlet. The amount of luteolin in each sample extract was measured using a preparative HPLC technique Results: Methanol was the best solvent, and the best extraction method was the reflex extraction method, based on HPLC results Conclusion: According to the results of HPLC, reflex was the superior method for extracting luteolin from V. pseudonegundo, and the optimum solvent was methanol. thus, advising using this approach in industry and future study.

Exploring in vitro and in silico Biological Activities of Calligonum Comosum and Rumex Vesicarius: Implications on Anticancer and Antibacterial Therapeutics

IntroductionThe adverse effects of clinically used anti-cancer medication and the rise in resistive micro-organisms have limited therapeutic options. Multiple anti-cancer drugs are derived from medicinal herbs which also have shown anti-bacterial effects. This study aimed to identify the optimal extraction solvent for detecting the cytotoxic and anti-bacterial effects of Calligonum comosum (C. Comosum) and Rumex vesicarius (R. Vesicarius) extracts. Additionally, the study aimed to identify active metabolites and assess their potential as future drug candidates for anti-cancer and anti-bacterial therapeutics. MethodsLeaves from both plants were extracted using ethanol, ethyl acetate, chloroform, and water. The cytotoxic effects of the extracts were tested on liver, colon, and breast cancer cell lines. Apoptosis was assessed using High Content Imaging (HCI) and the ApoTox triplex Glo assay. The anti-bacterial effects were determined using agar-well diffusion. Liquid chromatography-mass spectrometry (LC-MS) was used to tentatively identify the secondary metabolites. In silico computational studies were conducted to determine the metabolites' mode of action, safety, and pharmacokinetic properties. ResultsThe ethanolic extract of C. Comosum exhibited potent cytotoxicity on breast cancer cell lines, with IC50 values of 54.97 μg/mL and 58 μg/mL for KAIMRC2 and MDA-MB-231, respectively. It also induced apoptosis in colon and breast cancer cell lines. All tested extracts of C. Comosum and R. Vesicarius demonstrated anti-bacterial activity against Staphylococcus aureus and Escherichia coli. Seven active metabolites were identified, one of which is Kaempferol 3-O-Glucoside-7-O-Rhamnoside, which showed strong (predicted) anti-cancer activity. Kaempferol 3-O-Glucoside-7-O-Rhamnoside and Quercetin-3-O-Glucuronide also exhibited potential anti-bacterial effects on gram-positive and negative bacteria. ConclusionEthanol extraction of C. Comosum solubilizes active metabolites with potential therapeutic applications in cancer treatment and bacterial infections. Kaempferol 3-O-Glucoside-7-O-Rhamnoside, in particular, shows promise as a dual therapeutic drug candidate for further research and development to improve its efficacy, safety, and pharmacokinetic profile.

Determination of Active Ingredients, Mineral Composition and Antioxidant Properties of Hydroalcoholic Macerates of Vinca minor L. Plant from the Dobrogea Area.

In recent decades, new alternative therapies using drugs containing active ingredients of natural origin have been a hot topic for medical research. Based on the confirmed therapeutic potential of the Vinca minor plant, considered in the specialized literature to be of pharmaceutical interest, the purpose of this study is to determine the chemical and mineral composition of the Vinca minor plant grown in the Dobrogea area, with a view to its use in the formulation of dermal preparations. For this purpose, plant materials were collected from the mentioned area and hydroalcoholic macerates of different concentrations were obtained: 40%, 70% and 96% from leaves (F40, F70, F96) and stems (T40, T70, T96) of Vinca minor plant to determine the optimal extraction solvent. The hydroalcoholic macerates were analyzed via the HPLC method for the identification and quantification of the main bioactive compounds, and two methods were used to evaluate their antioxidant properties: the DPPH radical scavenging test and the photochemiluminescence method. HPLC analysis showed the presence of four indole alkaloids: vincamine, 1,2-dehydroaspidospermidine, vincaminoreine and eburnamonine. Vincamine was the alkaloid found in the highest concentration in Vinca leaves (2.459 ± 0.035 mg/100 g d.w.). The antioxidant activity of Vinca minor hydroalcoholic macerates showed values between 737.626-1123.500 mg GAE/100 g d.w (DPPH test) and 77.439-187.817 mg TE/100 g d.w (photochemiluminescence method). The concentrations of toxic metals Cd, Cu, Ni, Pb in dried leaves and stems of Vinca minor, determined by AAS, were below detection limits.

Quantitative analysis and survey of 9,10-anthraquinone contaminant in Chinese Liupao tea

Recently, 9,10-anthraquinone (AQ) contamination in Chinese Liupao tea has attracted much attention because the tea for export must meet the EU limit (10 µg kg−1). In this study, a method was developed in which the sample was extracted with n-hexane-acetone solution, then purified with Florisil adsorbent, detected by GC-MS/MS and contamination levels of AQ determined using an internal standard. This method was found to be more suitable for Liupao tea and other dark tea complex substrates than the QuEChERS procedure. The sample pre-treatment method was optimized with respect to extraction reagent and clean-up column adsorbent and n-hexane-acetone selected as the optimal extraction solvent. When the content of Florisil in the column was 1.0 g, the optimum clean-up was achieved. The new method reduced the limit of quantification (LOQ) of AQ to 10 μg kg−1, and accuracy was also further improved. The recovery of AQ-fortified tea samples containing 20–100 µg·kg−1 was 94.5–100.4%, and the relative standard deviation (RSD) was less than 1.3%. In a small survey, 98 Liupao tea samples on the market were tested by the new method. It was found that 61 samples were positive (occurrence rate 63.3%), and thus exceeded the EU limit (10 µg kg−1). This study also found that the contamination of AQ in Liupao tea increased with the length of ageing. The source of AQ in the Liupao tea ageing process will be the focus of further research.

Green Extraction of Phenolic Compounds from Lotus (Nelumbo nucifera Gaertn) Leaf Using Deep Eutectic Solvents: Process Optimization and Antioxidant Activity

Natural deep eutectic solvents (NDESs) were used to extract flavonoids and polyphenols from lotus (Nelumbo nucifera Gaertn.) leaves at the same time, and the extraction process was optimized to provide reference for the effective development and utilization of lotus leaves. The deep eutectic solvents (DESs) with the highest yield of flavonoids and polyphenols were screened out from 19 different NDES combinations. The response surface method was employed to optimize the extraction process. After a rational design, a lactic acid/glycerol (molar ratio 1:2) DES was chosen as the optimal extraction solvent, and the optimum extraction parameters were as follow: water content (29%), liquid–solid ratio (37:1 mL/g), extraction time (61 min), and extraction temperature (53 °C). Compared with traditional water extraction or ethanol extraction, it improved the yield of flavonoids (126.10 mg/g) and polyphenols (126.10 mg/g). By LC–MS analysis, 19 flavonoids or organic acid compounds with known compound structural formulae were identified in the DES extract of lotus leaves. By comparing the free radical scavenging ability and total reducing ability, the extraction of lotus leaves using the NDES method was superior to both ethanol extraction and water extraction. It is a green, environmentally friendly, and efficient extraction method for antioxidants from leaves of Nelumbo nucifera Gaertn.

Changes in nutritional, physicochemical, phytochemical composition and antioxidant potential of Mahonia nepalensis fruits during ripening

ABSTRACT The Himalayan region supports a rich diversity of edible fruit species that can cope with global food and nutritional security by providing dietary diversity, genetic backup for commercial species and economic sustainability. Among these, Mahonia nepalensis DC. (Family Berberidaceae) is a medicinally important plant species of Himalaya with delicious edible berry fruits. Fruits of the species remain unexplored, however, their content of nutrients and phytochemicals and antioxidant potential changed with the ripening process. The current study assessed variations in nutritional, physicochemical, and phytochemical composition and antioxidant potential during the four ripening stages. A significant (p < .05) and sequential change in morphological (length, diameter, fresh weight, and volume), physicochemical (juice, juice pH, pomace, moisture, and juice pomace ratio), nutritive phytochemicals (riboflavin, lycopene, β-carotene, and total carotenoids), and antioxidant potential of the species were observed among the ripening stages. Total phenolic, flavonoid, and flavonol content exhibited an initial decrease followed by a consistent increase; however, tannin content decreased with the ripening process. Phenolic content identified in fruits exhibited order of concentration as chlorogenic acid > caffeic acid > syringic acid > ferulic acid > p-coumaric acid, and among these, chlorogenic acid decreased significantly (p < .05) with fruit ripening. Higher total phenolic, flavonoid, flavonol, and tannin contents and antioxidant activity in acidified methanolic extract than in methanolic extract indicated the presence of considerable content of glycosides as compared to aglycones in fruits. Presence of high nutritive phytochemicals, antioxidant potential, optimized extraction solvent, suitable harvesting stage in the species might be utilized as alternative dietary resources, potential nutraceutical and post-harvest management of Mahonia nepalensis berries.

Optimization of green extraction process with natural deep eutectic solvent and comparative in vivo pharmacokinetics of bioactive compounds from Astragalus-Safflower pair

IntroductionNatural deep eutectic solvents (NaDESs) are promising not only in componential extraction, but also in drug delivery system due to their green and safe features. In this work, NaDESs were applied to extract bioactive components from Astragalus-Safflower pair, a classic traditional Chinese medicine combination. Furthermore, ready-to-use crude extracts were administrated to SD rats. MethodsTotal 9 NaDESs composed of food grade ingredients were screened for the extraction of representative 9 components (hydroxysafflor yellow A, anhydrosafflor yellow B, eleutheroside B, calycosin-7-O-glucoside, kaempferol-3-O-rutinoside, ononin, calycosin, astraganoside, and carthamin) from Astragalus-Safflower pair. Afterwards, genetic artificial neural network (GNN) was adopted for optimizing the ultrasound-assisted extraction process. After SD rats were orally administrated with the ready-to-use crude extracts extracted under the optimized conditions, the in vivo pharmacokinetic characteristics of 5 components were evaluated comprehensively from weight, gender, solvent and modeling surgery, under a well-established UPLC-MS/MS method. ResultsBetaine-Lactic acid (Bet-Lac) was eventually determined as the optimal extraction solvent for subsequent experiments. The optimal ultrasound assisted extraction process was as follows: 90 min of extraction time, 65 °C of temperature, 80% of Bet-Lac content and 50 mg/ml of solid-liquid ratio. Bet-Lac enhanced to varying degrees the bioavailability of analytes in normal and cerebral ischemia/reperfusion injured (CI/RI) rats in contrast with corresponding rats administrated with water extract groups (p < 0.05). Besides, the bioavailability of active components in CI/RI rat plasma was significantly lower than that in normal rats (p < 0.05), indicating pathological damage of CI/R had a significant impact on pharmacokinetic profile of compounds in rats. However, gender and body weight had no significant effects on the pharmacokinetic profile of bioactive components. ConclusionsNaDESs exhibited higher extraction efficiency than conventional solvents. And GNN is reliable to optimize the ultrasound assisted extraction process. This study supported the potential of non-toxic NaDESs as solvents for extraction process and drug delivery systems at the same time.

Применение газовой хромато-масс-спектрометрии для определения содержания хлорорганических соединений в химических реагентах

The possibilities of gas chromatography mass spectrometry for determining of organochlorine compounds content in chemical reagents are shown . The optimal operating conditions of the chromato mass spectrometer and the optimal solvent for extraction- isooctane were selected using the example of organochlorine compounds ( model mixture analysis. Calibration curves were constructed for each individual organochlorine compound at selected ion monitoring (SIM) mode. Different approaches to sample preparation based on dilution and/or extraction are proposed depending on the physico-chemical characteristics of chemical reagents. For the analysis of chemical reagents having a strong hydrocarbon background in the full ion current scanning mode, the identification of organochlorine compounds and subsequent quantitative determination were carried out by using mass fragmentograms. To estimate the efficiency of the technique, the completeness of extraction was assessed by adding a so-called "marker" to the working sample and evaluating the results by the value of the extraction degree.

Optimizing the extraction of phenolic antioxidants from date palm fruit by simplex-centroid solvent mixture design

Date palm (Phoenix dactylifera L.) fruits are rich in various bioactive compounds, such as phenolic acids, hydroxycinnamates, flavonoid glycosides, coumarins, alkaloids, and proanthocyanidin oligomers. The focus of this study was to develop a simplex-centroid mix design method to identify the most suitable mixture of solvents (water, acetone, and methanol) to extract bioactive compounds from date fruits. Three extraction solvents (water, methanol, and acetone) were investigated during this study to determine, total phenolic content (TPC), total flavonoid content (TFC), antioxidant activity (free radical DPPH) and ferric reduction ability (FRAP). The results showed that polar mixtures were effective in extracting antioxidant phenolics. The optimum solvent for extraction was Binary mixture water-acetone (50%) presenting TPC, TFC, DPPH and FRAP values of 502.88 mg GAE.100 g-1 DW, 206.23 mg QE.100 g−1 DW, 77 0.01% and 1688.66 μmol.100 g−1 respectively. The results also confirmed a strong correlation between the amount of polyphenols in a given extract and the antioxidant activities observed in the DPPH and FRAP assays. This study presents a pragmatic and efficient way to choose a solvent combination to extract polyphenols from date palm fruits.

Optimization of natural deep eutectic solvents extraction of flavonoids from Xanthoceras sorbifolia Bunge by response surface methodology

A green and efficient extraction of flavonoids from Xanthoceras sorbifolia Bunge by using ultrasound-assisted natural deep eutectic solvents combined with response surface methodology. Response surface methodology was used to optimize the extraction process. We aimed to test the scavenging ability of sixteen different NADESs and methanol extracts on DPPH and ABTS free radicals. The optimal extraction solvent was as follows: 1, 4-butanediol-acetic acid. With the best solvent the optimal extraction conditions were as follows: molar ratio 1:3, water content 33%, solid-liquid ratio 1:18 g mL−1 and extraction time 33 min. Under these conditions, the yields of (−)-epigallocatechin, catechin, epicatechin, dihydromyricetin, taxifolin and myricetin were 9.99, 1.38, 11.08, 6.53, 0.84 and 0.54 mg g−1, respectively. A total extraction yield of 30.37 mg g−1 was obtained. The IC50 values of DPPH and ABTS radical scavenging were 3.18 μg mL−1 and 0.51 mg mL−1, respectively. This study suggests that the extraction efficiency and antioxidant activity of 1, 4-butanediol-acetic acid were higher than traditional organic solvent methanol and have the advantages of environmental protection. The experiment provided a new method for the extraction of flavonoids from Xanthoceras sorbifolia Bunge.

Simultaneous Determination of 79 Polar and Non-Polar Polycyclic Aromatic Compounds in Airborne Particulate Matter by Gas Chromatography – Tandem Mass Spectrometry

Research on Polycyclic Aromatic Compounds (PACs) in the atmospheric environment has been mainly focused on the 16 EPA’s PAHs. Due to toxicological relevance and particular emission sources, there is a research need in broadening the scope of PACs analysis to include polar and semi-polar PACs in new analytical methods. Here, we describe a single GC-MS/MS method to simultaneously determine 79 polar, semi-polar and non-polar PACs. Temperature gradient and injection conditions were optimized. Optimal Multiple Reaction Monitoring (MRM) and pseudo-MRM mass transitions were searched to enhance the detection. PACs were extracted from particulate samples by Pressurized Liquid Extraction (PLE). The choice of the optimal extraction solvent was carefully evaluated. Instrumental LOQ were from 1 to 2 ng. The method was validated against linearity of the calibration, intra-day and inter-day variability, LOQ and recoveries. The analysis of a Diesel Particulate Matter Certified Reference Material enabled a firm method validation. The method was applied to PM10 samples from a residential parking lot. PACs total amount varied from 2.3 to 14 ng/m3. The most abundant PACs were phthalic anhydride, 1,8-naphthalic anhydride and benzo(b)fluoranthene. PAHs diagnostic ratios enabled the identification of fuel combustion and vehicular traffic as the main source of PACs.

Optimization of ultrasonic-assisted extraction model of Pinus koraiensis seed scales oil induced by tea saponin

Tea saponin was used for UAE of oil from Pinus koraiensis seed scales for the first time, and the extraction kinetic model was fitted and compared with that of traditional SE. Considering the relationship among the oil yield, proanthocyanidins content and solvent properties, ethanol was selected as the optimum extraction solvent. PBD and BBD were used to determine the optimal conditions: 63% aqueous ethanol solution, liquid-to-material ratio was 11:1 mL/g, ultrasonic power was 100 W, ultrasonic duration was 15 min, temperature was 45 °C, and the dose of tea saponin was 0.3%. Under the optimal conditions, the oil yield and proanthocyanidins content from P. koraiensis seed scales were 22.73 ± 0.42% and 3.04 mg/g ± 0.08%, respectively. The actual operating value was consistent with the theoretically predicted value. Comparison of the extraction kinetics model, oil components, physical and chemical properties, antioxidants, microstructure of oil residue, energy consumption and ecological emission characteristics of UAE and SE shows that UAE is a more advantageous technique.

Effects of Extraction Solvents on the Total Phenolic Content, Total Flavonoid Content, and Antioxidant Activity in the Aerial Part of Root Vegetables

The present study aimed to investigate the total phenolics, total flavonoids, and antioxidant activity in terms of the DPPH scavenging, reducing power, and H2O2 scavenging of the aerial parts of onion, white radish, red radish, carrot, and beet as affected by different extraction solvents. Generally, the aerial part of these vegetables has high antioxidant properties. Samples were extracted with methanol (100 and 70%), ethanol (100 and 70%), and water. Total phenolic content was highest when the samples were extracted using 100% methanol, while extraction with 100% ethanol yielded the highest total flavonoids. The highest DPPH activity and H2O2 scavenging values were obtained by extraction of the aerial plant parts with 70% ethanol, and the 70% methanol extract had the highest reducing power. Partial least regression (PLS) was performed to validate the optimum solvent for extraction of the antioxidants and their activity in each plant. The PLS indicated that there was a variation in the validation of the different extracts for each plant. The high antioxidant capacity of root vegetables, which is natural, indicates that they may have health and dietetic advantages for consumers.

Determination of free amino acids in Eriocheir sinensis by ultra-high performance liquid chromatography-high resolution mass spectrometry

游离氨基酸不仅是一类重要的营养物质,更与中华绒螯蟹独特的滋味和香味密切相关。对游离氨基酸含量进行测定,能为中华绒螯蟹产品的品质评价和风味研究提供有价值的信息。该工作通过优选提取溶剂、优化仪器测定参数,最终使用5%(v/v)高氯酸水溶液提取目标物,采用XDB-C18色谱柱(100 mm×4.6 mm, 1.7 μm),以0.1%(v/v)甲酸水溶液-乙腈为流动相进行梯度洗脱,在电喷雾正离子电离、选择离子扫描模式下进行检测,外标法定量,建立了超高效液相色谱-高分辨质谱(UHPLC-HRMS)测定中华绒螯蟹中17种游离氨基酸含量的方法。结果表明,17种氨基酸在10.0~200.0 mg/L范围内线性关系良好,相关系数(R2)≥0.9990,仪器检出限为0.3 mg/L,仪器定量限为1.0 mg/L。在中华绒螯蟹可食部分中按三水平进行加标回收试验,各目标物的回收率在78.4%~105.3%之间。通过对仪器和方法精密度进行评估,发现17种氨基酸测定仪器重复性的RSD≤4.2%,方法重复性试验的RSD≤5.2%,再现性试验的RSD≤11.4%,精密度数据均在合理范围内。利用该研究建立的检测方法对20个中华绒螯蟹样本进行了实际样品检测,总结了17种游离氨基酸在蟹肉、蟹膏、蟹黄中的分布特点,验证了该方法是一种前处理简便、选择性好、准确度高的检测技术。

Simultaneous determination of nine C4–C9 alkylphenols and bisphenol A in environmental water using gas chromatography-mass spectrometry

A liquid-liquid extraction method combined with derivatization and gas chromatography-mass spectrometry (GC-MS) was developed for the simultaneous determination of nine C4–C9 alkylphenols (APs, including 4- tert -butylphenol, 4- n -butylphenol, 4- n -pentylphenol, 4- n -hexylphenol, 4- n -heptylphenol, 4- n -octylphenol, 4- tert -octylphenol, 4- n -nonylphenol and 4-nonylphenol) and bisphenol A (BPA) in environmental water. The derivatization time, extraction solvent, volume of extraction solvent, extraction time, extraction number, pH value of water, salt content, and concentration degree were optimized. These target compounds were quantified by internal standard method. The experimental result showed that the optimal extraction time, number, solvent volume, pH value and salt content were 5 min, 2, 30 mL, about 2 and 10 g/L, respectively, and derivatization time was 1 h at room temperature. Dichloromethane was selected as the extraction solvent and concentrated to 0.5 mL in the process of concentration. The developed method showed good linearity ( R 2 > 0.995), low limit of detection (LOD, 0.002–0.006 μg/L), and satisfactory recoveries (68.0%–122%) and low relative standard deviation (0.67%–13.7%). The method was used to analyse groundwater, surface water, seawater and sewage samples in Dongying City located at Yellow River Estuary, and 4-nonylphenol and BPA in these water samples were detected. However, these measured values were below their restrictive values of relevant directives at home and abroad. A diagram shows a liquid-liquid extraction combined with derivatization and gas chromatography-mass spectrometry (GC-MS) method for the rapid determination of C4-C9 alkylphenols (4- tert -butylphenol, 4- n -butylphenol, 4- n -pentylphenol, 4- n -hexylphenol, 4- n -heptylphenol, 4- n -octylphenol, 4- tert -octylphenol, 4- n -nonylphenol and 4-nonylphenol) and bisphenol A in the environmental water.

Temperature-responsive deep eutectic solvent as eco-friendly and recyclable media for the rapid assessment of pyrethroid pesticide residues in surface soil sample

In the modern agricultural model, more and more attention has been paid to green production and sustainable agriculture practices. In this study, a simple and eco-friendly extraction method for the rapid assessment of nine different pyrethroid pesticides in surface soil samples was developed by the temperature-responsive deep eutectic solvent-based ultrasound assisted extraction. Three different temperature-responsive deep eutectic solvent systems of various classes were prepared to extract pyrethroid pesticides from spiked soil samples. The total spiked recovery displayed that temperature-responsive deep eutectic solvent composed of ethanolamine and o-cresol with molar ratio 1:1 was the optimum extraction solvent for temperature-responsive deep eutectic solvent-based ultrasound assisted extraction procedure. Based on Box-Behnken Design, the maximum extraction recovery (%) of total pyrethroid pesticides was 94.23% under the following conditions: extraction temperature of 68 °C, extraction time of 35 min, and solid–liquid ratio of 21 mg/mL. Meaningfully, the extraction recovery of pyrethroid pesticides was still more than 80% after fifth cycles of temperature-responsive deep eutectic solvent, demonstrating that temperature-responsive deep eutectic solvent could be repeatedly used. The detection results of actual soil samples indicated that the pyrethroid pesticide residues (8.42–28.72 μg/kg) in vineyard region were the most serious, which may be due to the high incidence of insect pests and the abuse of pesticides. The temperature-responsive deep eutectic solvent-based ultrasound assisted extraction method with the advantages of fast, trace, and high efficiency could be successfully applied to pyrethroid pesticide residues analysis in surface soil samples.

Simultaneous determination of trichothecene mycotoxins in cereals by LC-MS/MS.

This study was designed to determine the residual trichothecene mycotoxins in cereal samples. The optimal solvent for extraction was 84% (v/v) aqueous acetonitrile with 1% (v/v) formic acid. The best performing clean-up method was dispersive-solid phase with a mixture octadecyl silica and primary-secondary amine. The recoveries for the studied mycotoxins ranged from 83.3 to 92.8%. The methodology was successfully applied for monitoring 100 cereal samples obtained from a Korean market. The bean sample were found to be co-contamination with deoxynivalenol and HT-2 toxin. Deoxynivalenol possessed the highest detection freauency (4/100) and amount (727.38µg/kg) among the trichothecene mycotoxins. The hazard index was less than 1.0 for all the observed mycotoxins in all cereal samples except one white rice sample (1.2681). This results indicated that periodic risk assessments of trichothecene mycotoxin through cereal intake are necessary for the health and safety.

Analysis and Clinical Application of Polyunsaturated Fatty Acids in Human Serum Using One-step Extraction and Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

Omega-3 and omega-6 fatty acids are reported to alleviate various inflammatory reactions such as asthma, chronic obstructive pulmonary disease, rheumatoid arthritis, and inflammatory bowel disease. We have developed a new method for their quantitation in serum, utilizing ultra-high-performance liquid chromatography-electrospray ionizationtandem mass spectrometry (UHPLC-ESI-MS/MS) in multiple reaction monitoring (MRM) mode, under negative ionization. MRM transitions were detected for five omega fatty acids, as follows: α-linolenic acid, m/z=277.20→277.20; eicosapentaenoic acid, m/z=301.10→257.30; docosahexaenoic acid, m/z=327.00→283.15; arachidonic acid, m/z=303.20→259.25; docosapentaenoic acid, m/z=329.10→285.25. After comparing several different solvents, we selected butanol:methanol (1:1, v/v) as the optimal extraction solvent. Chromatographic separations were carried out using an Acclaim RSLC 120 C18 column (150×2.1 mm, 2.2 μm) at 40oC. For the mobile phase, solvent A consisted of water containing 5% acetonitrile and 5% methanol, and solvent B consisted of methyl tert-butyl ether:acetonitrile:methanol (10:20:70, v/v/v) containing 2.5 mM ammonium acetate. The calibration curve showed excellent linearity within the range of 0.01-20 μg/mL (R2=0.9996-0.9999). The analytical method was validated and shown to have excellent sensitivity (LOD; 0.001-0.005 μg/mL, LOQ; 0.01-0.2 μg/mL), making it suitable for targeted analyses of omega fatty acids. Recovery ranged from 78.0 to 103.9% (RSD 0.5-5.6%). This new method uses relatively small amounts of serum and extraction solvent and is expected to be suitable for analysis of various clinical specimens, such as plasma, urine, and cerebrospinal fluid.

Optimal delipidation solvent to secure extracellular matrix from human perirenal adipose tissue.

The objective of this study was to select the optimal delipidation solvent for preparation of human perirenal adipose tissue-derived extracellular matrix (ECM). Human perirenal adipose tissue can be obtained in large amounts during surgery, and it can be an alternative source of human ECM. Delipidation is an essential procedure for the ECM preparation, because lipid strongly inhibits regeneration of target tissue. Isopropanol has been widely used as a delipidation solvent for adipose tissue. However, because adipose tissue is mostly composed of nonpolar lipid, a nonpolar solvent might be more effective for delipidation. We evaluated the delipidation efficiency of acetone, chloroform, methanol, ether, ethanol, isopropanol, water, chloroform/methanol, ethanol/heptane, ether/methanol, hexane/ethanol, and butanol/methanol solvents for ECM extraction from human perirenal adipose tissue. Among them, acetone-treated adipose tissue showed the greatest delipidation efficiency (93.05%), significantly lower residual DNA content, and the greatest residual collagen concentration (42.49 ± 0.05 μg/g). In addition, acetone-treated tissue also had well-preserved ultrastructure with high porosity and significantly low in vitro cytotoxicity. These results suggested that acetone may be an optimal delipidation solvent for extraction of ECM from human perirenal adipose tissue.