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

被引：2

作者：

Dmitrieva, E., V ^{[1
]}

Temerdashev, A. Z. ^{[1
]}

Osipova, A. K. ^{[1
]}

机构：

[1] Kuban State Univ, Krasnodar 350040, Russia

来源：

JOURNAL OF ANALYTICAL CHEMISTRY | 2021年 / 76卷 / 11期

关键词：

steroid hormones; DLLME; urine; derivatization; hydroxylamine; HPLC with mass-spectrometric detection; EXPERIMENTAL-DESIGN; STEROID-HORMONES; LC-MS/MS; DERIVATIZATION; QUANTIFICATION; OPTIMIZATION; SENSITIVITY; EXTRACTION; PLASMA; SERUM;

D O I：

10.1134/S1061934821110034

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

A method is proposed for the determination of some ketosteroids in human urine, including enzymatic hydrolysis using beta-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 degrees 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.

引用

收藏

页码：1305 / 1311

页数：7

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