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使用粒子束接口将液相色谱与负离子化学电离质谱联用同时测定生物流体中的倍氯米松、倍氯米松单丙酸酯和倍氯米松二丙酸酯。

Simultaneous determination of beclomethasone, beclomethasone monopropionate and beclomethasone dipropionate in biological fluids using a particle beam interface for combining liquid chromatography with negative-ion chemical ionization mass spectrometry.

作者信息

Girault J, Istin B, Malgouyat J M, Brisson A M, Fourtillan J B

机构信息

CEMAF s.a., Poitiers, France.

出版信息

J Chromatogr. 1991 Mar 8;564(1):43-53. doi: 10.1016/0378-4347(91)80068-n.

Abstract

A new simple and sensitive assay has been developed for the simultaneous quantitative measurement of beclomethasone dipropionate and its hydrolysis products in human plasma and urine. Beclomethasone 17.21-dipropionate, beclomethasone 17-monopropionate, beclomethasone and the internal standard, dexamethasone 21-acetate, were measured by combined liquid chromatography and negative-ion chemical ionization mass spectrometry with methane as the reagent gas. A particle beam interface from Hewlett Packard was used. Under mild operating conditions, abundant and stable characteristic high-mass ions were generated in the ion source of the mass spectrometer by a resonance electron-capture mechanism. The fast extraction procedure requires 1 ml of plasma or urine, and the quantification limit of the method is 1 ng ml-1 for the three tested compounds.

摘要

已开发出一种新的简单且灵敏的测定方法,用于同时定量测定人血浆和尿液中丙酸倍氯米松及其水解产物。采用液相色谱与负离子化学电离质谱联用,以甲烷作为反应气,测定丙酸倍氯米松、17-单丙酸倍氯米松、倍氯米松以及内标地塞米松21-乙酸酯。使用了惠普公司的粒子束接口。在温和的操作条件下,通过共振电子捕获机制,在质谱仪的离子源中产生了丰富且稳定的特征高质量离子。快速提取程序需要1毫升血浆或尿液,该方法对三种被测化合物的定量限为1纳克/毫升。

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