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液相色谱-串联质谱法测定硫酸脱氢表雄酮方法的建立。

Development of a method for the measurement of dehydroepiandrosterone sulphate by liquid chromatography-tandem mass spectrometry.

作者信息

Chadwick C A, Owen L J, Keevil B G

机构信息

Clinical Biochemistry Department, Wythenshawe Hospital, Southmoor Road, Wythenshawe, Manchester M23 9LT, UK.

出版信息

Ann Clin Biochem. 2005 Nov;42(Pt 6):468-74. doi: 10.1258/000456305774538175.

DOI:10.1258/000456305774538175
PMID:16259799
Abstract

BACKGROUND

Dehydroepiandrosterone sulphate (DHEAS) is a steroid that is increasingly being recognized as a potential drug of abuse in many countries. This is due to its reputation as a hormone that may be able to retard the ageing process. The measurement of DHEAS is useful in the diagnosis of medical conditions such as congenital adrenal hyperplasia and polycystic ovary syndrome. Thus, a liquid chromatography-tandem mass spectrometry method has been developed to determine DHEAS concentrations in human serum.

METHOD

The chromatography was performed using a Waters 2795 Alliance HT LC system coupled to a Mercury Fusion-RP column fitted with a SecurityGuard column.

RESULTS

DHEAS and the internal standard, deuterated DHEAS, both had a retention time of 1.5 min. The transition determined by the Micromass Quattro tandem mass spectrometer for DHEAS was m/z 367.3>4 96.7 and for the internal standard m/z 369.3>96.6. The method was linear up to 20 micromol/L; the lower limit of detection and the lower limit of quantitation were both 1 micromol/L. The intra- and interassay imprecision were <11% over a concentration range of 1-18 micromol/L for the in-house quality control and <12% for the intra- and interassay imprecision for the Bio-Rad Lyphocheck QC.

CONCLUSION

The measurement of DHEAS by liquid chromatography-tandem mass spectrometry is robust and has a simple sample preparation procedure with a rapid cycle time of only 4 min.

摘要

背景

硫酸脱氢表雄酮(DHEAS)是一种类固醇,在许多国家越来越被视为一种潜在的滥用药物。这是因为它作为一种可能能够延缓衰老过程的激素而闻名。DHEAS的测量对于先天性肾上腺增生和多囊卵巢综合征等医学病症的诊断很有用。因此,已开发出一种液相色谱 - 串联质谱法来测定人血清中的DHEAS浓度。

方法

使用与配备有保安柱的Mercury Fusion - RP柱相连的Waters 2795 Alliance HT LC系统进行色谱分析。

结果

DHEAS和内标氘代DHEAS的保留时间均为1.5分钟。Micromass Quattro串联质谱仪测定的DHEAS的跃迁为m/z 367.3>496.7,内标的跃迁为m/z 369.3>96.6。该方法在高达20微摩尔/升的范围内呈线性;检测下限和定量下限均为1微摩尔/升。对于内部质量控制,在1 - 18微摩尔/升的浓度范围内,批内和批间不精密度均<11%,对于Bio - Rad Lyphocheck QC,批内和批间不精密度<12%。

结论

通过液相色谱 - 串联质谱法测量DHEAS性能稳定,样品制备程序简单,循环时间仅4分钟。

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