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使用键合相苯基硼酸柱和毛细管气相色谱-负离子化学电离质谱法测定尿中2,3-二去甲血栓素B2和血栓素B2

Measurement of urinary 2,3-dinor-thromboxane B2 and thromboxane B2 using bonded-phase phenylboronic acid columns and capillary gas chromatography--negative-ion chemical ionization mass spectrometry.

作者信息

Lawson J A, Brash A R, Doran J, FitzGerald G A

出版信息

Anal Biochem. 1985 Nov 1;150(2):463-70. doi: 10.1016/0003-2697(85)90536-6.

DOI:10.1016/0003-2697(85)90536-6
PMID:4091270
Abstract

The use of bonded-phase phenylboronic acid columns to selectively extract 2,3-dinor-thromboxane B2 and thromboxane B2 from urine is reported. The compounds were first derivatized as the methoxime and then applied to the phenylboronic acid columns. Subsequent purification by thin-layer chromatography and derivatization to the pentafluorobenzyl ester, trimethylsilyl ether followed by capillary gas chromatography-negative-ion chemical ionization mass spectrometry, monitoring specific ions, allows quantitation in the low-picogram/milliliter range. In healthy male volunteers, the median excretions of 2,3-dinor-thromboxane B2 and thromboxane B2 were 10.3 ng/h (range, 4.5-24 ng/h) and 2.8 ng/h (range, 0.5-7.3 ng/h), respectively. The method offers a noninvasive, specific approach to the study of thromboxane synthesis and platelet function in man. It is much less labor intensive than currently available methods employing electron-impact chromatography-mass spectrometry.

摘要

据报道,使用键合相苯基硼酸柱从尿液中选择性提取2,3-二去甲血栓素B2和血栓素B2。这些化合物首先被衍生化为甲氧肟,然后应用于苯基硼酸柱。随后通过薄层色谱法进行纯化,并衍生化为五氟苄酯、三甲基硅醚,接着进行毛细管气相色谱-负离子化学电离质谱分析,监测特定离子,可在低皮克/毫升范围内进行定量。在健康男性志愿者中,2,3-二去甲血栓素B2和血栓素B2的排泄中位数分别为10.3纳克/小时(范围为4.5 - 24纳克/小时)和2.8纳克/小时(范围为0.5 - 7.3纳克/小时)。该方法为研究人体血栓素合成和血小板功能提供了一种非侵入性的、特异性的方法。它比目前使用电子轰击色谱-质谱联用的方法所需的劳动强度小得多。

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