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前列腺素和血栓素乙酰衍生物的高效液相色谱 - 热喷雾质谱分析

High-performance liquid chromatography-thermospray mass spectrometry of prostaglandin and thromboxane acetyl derivatives.

作者信息

Yamane M, Abe A

机构信息

Department of Biochemistry, Tokyo Medical College, Japan.

出版信息

J Chromatogr. 1991 Jul 17;568(1):11-24. doi: 10.1016/0378-4347(91)80336-b.

Abstract

A quantitative analysis of prostaglandin-related substances has been developed. Hydroxyl groups of prostaglandin and thromboxane were acetylated by acetic anhydride, the mixture was partially purified on a Sep-Pak C18 cartridge and analysed by high-performance liquid chromatography combined with thermospray mass spectrometry. Using this method, twenty kinds of prostaglandin derivative could be detected simultaneously within 11 min on a selected-ion monitoring detection chromatogram without a gradient system. Generally, the base ion, [M + H - n(60)]+, is produced through elimination of acetic acid (n = number of the hydroxyl group of prostaglandin or thromboxane). The detection limit for these derivatives was ca. 0.2 pmol at the levels of prostaglandin-related substances prior to derivatization. They could be analysed in the range 0.5-10 pmol. The assay was successfully applied to prostaglandin-related substances in human seminal fluid and rat brain.

摘要

已开发出一种前列腺素相关物质的定量分析方法。前列腺素和血栓素的羟基用乙酸酐进行乙酰化,混合物在Sep-Pak C18柱上进行部分纯化,然后通过高效液相色谱结合热喷雾质谱进行分析。使用该方法,在选定离子监测检测色谱图上无需梯度系统即可在11分钟内同时检测到20种前列腺素衍生物。一般来说,基峰离子[M + H - n(60)]+是通过消除乙酸(n =前列腺素或血栓素羟基的数量)产生的。这些衍生物在衍生化前前列腺素相关物质水平下的检测限约为0.2皮摩尔。它们可在0.5 - 10皮摩尔范围内进行分析。该测定法已成功应用于人类精液和大鼠脑中的前列腺素相关物质分析。

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