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采用 DLLME 和 UHPLC-HRMS 检测法对人尿中甾体激素的定量分析。

Quantification of steroid hormones in human urine by DLLME and UHPLC-HRMS detection.

机构信息

Department of Analytical Chemistry, Kuban State University, 149 Stavropolskaya St., Krasnodar 350040, Russia.

Department of Analytical Chemistry, Kuban State University, 149 Stavropolskaya St., Krasnodar 350040, Russia.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2020 Nov 30;1159:122390. doi: 10.1016/j.jchromb.2020.122390. Epub 2020 Oct 6.

DOI:10.1016/j.jchromb.2020.122390
PMID:33126074
Abstract

A procedure for the quantification of steroid hormones of various classes in human urine (androgens, estrogens, progestins, corticosteroids) has been described consisting of sample preparation by means of dispersive liquid-liquid extraction after enzymatic hydrolysis with β-glucuronidase from E. Coli followed by ultra-high performance liquid chromatography-high resolution mass spectrometry (quadrupole time-of-flight) detection. Both one-variable-at-a-time and multivariate approaches (full factorial and Box-Behnken designs) were applied to optimize sample preparation conditions. The procedure was validated using synthetic urine in the concentration range of 0.25-500 ng/mL. Then, it was applied to the analysis of real urine samples and the results were compared with those of a common liquid-liquid extraction procedure. The results obtained proved its applicability to the quantification of steroid hormones in human urine with high sensitivity and accuracy.

摘要

已经描述了一种用于定量分析人尿中各种甾体激素(雄激素、雌激素、孕激素、皮质类固醇)的方法,该方法包括通过酶解(使用来自大肠杆菌的β-葡萄糖醛酸酶)和分散液-液萃取进行样品制备,然后进行超高效液相色谱-高分辨率质谱(四极杆飞行时间)检测。采用单变量法和多变量法(全因子和 Box-Behnken 设计)对样品制备条件进行了优化。该方法在 0.25-500 ng/mL 的浓度范围内使用合成尿液进行了验证。然后,将其应用于实际尿液样品的分析,并将结果与常用的液-液萃取方法进行了比较。结果表明,该方法具有高灵敏度和准确性,适用于人尿中甾体激素的定量分析。

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