scholarly journals Synergistic Combination of Facile Thiol-Maleimide Derivatization and Supramolecular Solvent-Based Microextraction for UHPLC–HRMS Analysis of Glutathione in Biofluids

2021 ◽  
Vol 9 ◽  
Author(s):  
Mengmeng Yan ◽  
Feng Gao ◽  
Meng Chen ◽  
Qi Hu ◽  
Yuqin Yang ◽  
...  
Keyword(s):  
High Performance ◽  
High Resolution Mass Spectrometry ◽  
High Sensitivity ◽  
Clinical Diagnostics ◽  
Critical Parameters ◽  
Extraction Solvent ◽  
Dispersing Agent ◽  
Supramolecular Solvent ◽  
Dispersive Liquid Liquid Microextraction

Glutathione (GSH) is the most abundant non-protein thiol in biofluids, enabling diverse physiological functions. Among the proposed methods for GSH detection, ultra-high-performance liquid chromatography (UHPLC) coupled with high-resolution mass spectrometry (HRMS) has the advantages of high sensitivity and efficiency. In this study, a novel analytical method was developed for the determination of GSH using supramolecular solvent (SUPRAS)-based dispersive liquid–liquid microextraction (DLLME) and UHPLC–HRMS. N-Laurylmaleimide was dissolved in tetrahydrofuran, which served three functions: 1) precipitate the proteins present in the biofluid sample, 2) provide a reaction environment for derivatization, and 3) enable the use of SUPRAS as the dispersing agent. Critical parameters were optimized based on single factor testing and response surface methodology. The established method was validated in terms of linearity, accuracy, precision, and successful quantitative analysis of GSH in saliva, urine, and plasma samples. Experimental results showed that SUPRAS as an extraction solvent was particularly suitable for the extraction of GSH from complex matrices. The current study provides a useful tool for accurate measurements of GSH concentrations, which could potentially be used for clinical diagnostics.

scholarly journals Determination of Ketosteroids in Human Urine Using Dispersive Liquid-Liquid Microextraction and Ultra High-Performance Liquid Chromatography-High Resolution Mass Spectrometry

2021 ◽  
Vol 76 (11) ◽  
pp. 1305-1311
Author(s):  
E. V. Dmitrieva ◽  
A. Z. Temerdashev ◽  
A. K. Osipova
Keyword(s):  
Mass Spectrometry ◽  
Human Urine ◽  
High Performance ◽  
High Resolution Mass Spectrometry ◽  
High Sensitivity ◽  
Reversed Phase ◽  
Flight Mass Spectrometry ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

Abstract A method is proposed for the determination of some ketosteroids in human urine, including enzymatic hydrolysis using β-glucuronidase from E. coli followed by dispersive liquid-liquid microextraction, derivatization of analytes with hydroxylamine, and detection by reversed-phase ultra-HPLC–quadrupole time-of-flight mass spectrometry. Optimization of extraction and derivatization conditions of the studied compounds made it possible to find that the highest recoveries were achieved using an acetone–chloroform mixture as a dispersant and an extractant, and the completeness of the derivatization reaction was achieved by thermostating the sample at 70°C for 90 min. The proposed method has high sensitivity (limits of detection in the range of 0.1–0.25 ng/mL) and a wide linearity range.

Coating Quartz Arc Tube with Polycrystalline Alumina for High Intensity Discharge Lamps

2013 ◽  
Vol 718-720 ◽  
pp. 219-222
Author(s):  
Jia Qi Ju ◽  
Zhong Hang Wu ◽  
Zhen Liu Chen ◽  
Zhi Jiang He ◽  
Long He ◽  
...  
Keyword(s):  
High Performance ◽  
Solid Phase ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Polycrystalline Alumina ◽  
Extraction Solvent ◽  
Chromatography Tandem Mass Spectrometry ◽  
Dispersing Agent ◽  
Liquid Chromatography Tandem Mass

This research developed and optimized the methods for simultaneous determination of tetracycline (TCs), macrolide (MLs) and sulfonamide (SAs) antibiotics in soils using accelerated solvent extraction (ASE)- solid-phase extraction (SPE)-high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Methanol-citric acid (pH=4.7) was used as extraction solvent, diatomite (washed by EDTA) was used as dispersing agent. Firstly, soil was extracted by ASE with the parameter conditions: pressure 1500 psi, temperature 70°C, static 10 min, 1 circle, then pre-concentration by SPE and followed by HPLC-MS/MS analysis. Recovery was 86.3%~97.4% for SAs, 67.3%~87.4% for TCs and 68.4%~78.3% for MLs. RSD < 9 % and r > 0.99. Limits of detection (LOD) was 0.5~0.9 ug/kg for SAs, 0.2~1.1 ug/kg for TCs and 0.2~0.3 ug/kg for MLs. This method determined 9 kinds of antibiotics within 15 min, the determination accuracy can meet the requirements of actual analysis.

Simultaneous Determination of Four Plant Hormones in Soil by Ultrasound-Assisted Ionic Liquid Based Dispersive Liquid-Liquid Microextraction

2014 ◽  
Vol 675-677 ◽  
pp. 181-184 ◽  
Author(s):  
Gui Qi Huang ◽  
She Ying Dong ◽  
Zhen Yang ◽  
Ting Lin Huang
Keyword(s):  
Ionic Liquid ◽  
Plant Hormones ◽  
High Performance ◽  
Extraction Solvent ◽  
Target Analytes ◽  
Relative Standard ◽  
Ultrasound Assisted ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

An ultrasound-assisted ionic liquid based dispersive liquid-liquid microextraction (UA-IL-DLLME) was developed for the determination of four plant hormones (6-benzyladenine (6-BA), kinetin (6-KT), 2, 4-dichlorophenoxy acetic acid (2, 4-D) and uniconazole (UN)) in soil, using high performance liquid chromatography (HPLC)-diode array detection (DAD). Several important parameters including the type and volume of extraction solvent, the volume of disperser solvent, ultrasound time, pH of the solution and salt effect were studied and optimized. Under optimum conditions, the limits of detections (LODs) for the target analytes were in the range of 0.002-0.01 μg g-1. And satisfactory recoveries of the target analytes in the soil samples were 79.3-96.7 %, with relative standard deviations (RSD, n=5) that ranged from 4.3 to 6.7%.

Rational design of an ionic liquid dispersive liquid–liquid micro-extraction method for the detection of organophosphorus pesticides

The Analyst ◽  
2019 ◽  
Vol 144 (6) ◽  
pp. 2166-2172 ◽  
Author(s):  
Dingkun Lu ◽  
Chang Liu ◽  
Jingjing Deng ◽  
Xinguang Zhou ◽  
Guoyue Shi ◽  
...  
Keyword(s):  
Ionic Liquid ◽  
Extraction Method ◽  
High Performance ◽  
Rational Design ◽  
Organophosphorus Pesticides ◽  
Extraction Solvent ◽  
Sensitive Determination ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

In this study, a functionalized ionic liquid (IL), [MimCH2COOCH3][NTf2] was rationally designed and explored as an extraction solvent in dispersive liquid–liquid microextraction (DLLME) combined with ultra-high performance liquid chromatography (UHPLC) for the sensitive determination of organophosphorus pesticides (OPs).

Determination of Selected Phthalates in Some Commercial Cosmetic Products by HPLC-UV

2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural
Keyword(s):  
High Performance ◽  
Phthalate Esters ◽  
High Sensitivity ◽  
Hplc Method ◽  
Cosmetic Products ◽  
Limit Of Quantification ◽  
Nail Polish ◽  
Accuracy And Precision ◽  
Butyl Phthalate

Aim and scope: Due to the serious toxicological risks and their widespread use, quantitative determination of phthalates in cosmetic products have importance for public health. The aim of this study was to develop a validated simple, rapid and reliable high-performance liquid chromatography (HPLC) method for the determination of phthalates which are; dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), di-n-butyl phthalate (DBP), di(2- ethylhexyl) phthalate (DEHP), in cosmetic products and to investigate these phthalate (PHT) levels in 48 cosmetic products marketing in Sivas, Turkey. Materials and Methods: Separation was achieved by a reverse-phase ACE-5 C18 column (4.6 x 250 mm, 5.0 μm). As the mobile phase, 5 mM KH2PO4 and acetonitrile were used gradiently at 1.5 ml min-1. All PHT esters were detected at 230 nm and the run time was taking 21 minutes. Results: This method showed the high sensitivity value the limit of quantification (LOQ) values for which are below 0.64 μg mL-1 of all phthalates. Method linearity was ≥0.999 (r2). Accuracy and precision values of all phthalates were calculated between (-6.5) and 6.6 (RE%) and ≤6.2 (RSD%), respectively. Average recovery was between 94.8% and 99.6%. Forty-eight samples used for both babies and adults were successfully analyzed by the developed method. Results have shown that, DMP (340.7 μg mL-1 ±323.7), DEP (1852.1 μg mL-1 ± 2192.0), and DBP (691.3 μg mL-1 ± 1378.5) were used highly in nail polish, fragrance and cream products, respectively. Conclusion: Phthalate esters, which are mostly detected in the content of fragrance, cream and nail polish products and our research in general, are DEP (1852.1 μg mL-1 ± 2192.0), DBP (691.3 μg mL-1 ± 1378.5) and DMP (340.7 μg mL-1 ±323.7), respectively. Phthalates were found in the content of all 48 cosmetic products examined, and the most detected phthalates in general average were DEP (581.7 μg mL-1 + 1405.2) with a rate of 79.2%. The unexpectedly high phthalate content in the examined cosmetic products revealed a great risk of these products on human health. The developed method is a simple, sensitive, reliable and economical alternative for the determination of phthalates in the content of cosmetic products, it can be used to identify phthalate esters in different products after some modifications.

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