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一种新型的超高效超临界流体色谱串联质谱法对外周类固醇的靶向分析。

A Novel Targeted Analysis of Peripheral Steroids by Ultra-Performance Supercritical Fluid Chromatography Hyphenated to Tandem Mass Spectrometry.

机构信息

Department of Chemistry - Biomedical Center, Analytical Chemistry, Uppsala University, Box 599, Uppsala, 75124, Sweden.

出版信息

Sci Rep. 2018 Nov 19;8(1):16993. doi: 10.1038/s41598-018-35007-0.

DOI:10.1038/s41598-018-35007-0
PMID:30451874
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6242962/
Abstract

Ultra-performance supercritical fluid chromatography-tandem mass spectrometry (UPSFC-MS/MS) is an alternative method for steroid analysis. Continuous development of analytical methodologies for steroid profiling is of major importance in the clinical environment to provide useful and more comprehensive data. The aim of this study was to identify and quantify a large number of endogenous steroids from the four major classes (estrogens, androgens, progestogens and corticosteroids) simultaneously within a short analytical time. This novel UPSFC-MS/MS method with electrospray in positive ionisation (ESI+) mode is robust, selective and present sufficiently high sensitivity to profile nineteen steroids in 50 µL human plasma. Under optimised conditions, nineteen different steroids were separated with high efficiency in the multiple reaction monitoring (MRM) mode. The linearity of the method was good with correlation coefficients (R) in the range of 0.9983-0.9999 and with calibration range from 0.05-500 ng/mL in human plasma. The intraday and interday precision of the method, as RSD, was less than 15%. The accuracy of the nineteen analytes varied between 80 to 116%. Finally, the novel method was successfully applied for the determination of nineteen steroids within 5 minutes providing the possibility to use it for research as well as routine healthcare practice.

摘要

超高效超临界流体色谱-串联质谱法(UPSFC-MS/MS)是一种替代的类固醇分析方法。在临床环境中,不断开发类固醇分析方法对于提供有用且更全面的数据至关重要。本研究的目的是在短分析时间内同时鉴定和定量来自四大类(雌激素、雄激素、孕激素和皮质类固醇)的大量内源性类固醇。该新型 UPSFC-MS/MS 方法采用正离子化(ESI+)模式的电喷雾,具有稳健性、选择性,并且具有足够高的灵敏度,可在 50µL 人血浆中对 19 种类固醇进行分析。在优化条件下,19 种不同的类固醇在多重反应监测(MRM)模式下以高效率分离。该方法的线性良好,相关系数(R)在 0.9983-0.9999 范围内,校准范围为 0.05-500ng/mL。该方法的日内和日间精密度(RSD)小于 15%。19 种分析物的准确度在 80%至 116%之间变化。最后,该新方法成功地用于 5 分钟内测定 19 种类固醇,为其在研究以及常规医疗保健实践中的应用提供了可能性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/75db/6242962/ded2313223c2/41598_2018_35007_Fig3_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/75db/6242962/619381e90da5/41598_2018_35007_Fig1_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/75db/6242962/ece820671a8c/41598_2018_35007_Fig2_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/75db/6242962/ded2313223c2/41598_2018_35007_Fig3_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/75db/6242962/619381e90da5/41598_2018_35007_Fig1_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/75db/6242962/ece820671a8c/41598_2018_35007_Fig2_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/75db/6242962/ded2313223c2/41598_2018_35007_Fig3_HTML.jpg

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