DETERMINATION OF 6-KETO-PGF1-ALPHA, 2,3-DINOR-6-KETO-PGF1-ALPHA, THROMBOXANE-B2, 2,3-DINOR-THROMBOXANE-B2, PGE2, PGD2 AND PGF2-ALPHA IN HUMAN URINE BY GAS-CHROMATOGRAPHY NEGATIVE-ION CHEMICAL IONIZATION MASS-SPECTROMETRY

被引：21
|
作者：
WEBER, C [1 ]
HOLLER, M [1 ]
BEETENS, J [1 ]
DECLERCK, F [1 ]
TEGTMEIER, F [1 ]
机构：
[1] JANSSEN RES FDN, B-2340 BEERSE, BELGIUM
来源：
JOURNAL OF CHROMATOGRAPHY-BIOMEDICAL APPLICATIONS | 1991年 / 562卷 / 1-2期
关键词：
D O I：
10.1016/0378-4347(91)80611-F
中图分类号：
O65 [分析化学];
学科分类号：
070302 ; 081704 ;
摘要：
A method for quantification of 6-keto-PGF1-alpha, TXB2, 2,3-dinor TXB2, PGE2, PGD2 and PGF2-alpha in human urine samples, using gas chromatography-negative ion chemical ionization mass spectrometry, is described. Deuterated analogues were used as internal standards. Methoximation was carried out in urine samples which were subsequently applied to phenylboronic acid cartridges, reversed-phase cartridges and thin-layer chromatography. The eluents were further derivatized to pentafluorobenzyl ester trimethylsilyl ethers for final quantification by gas chromatography-mass spectrometry. The overall recovery was 77% for tritiated 6-keto-PGF1alpha and 55% for tritiated TXB2. Urinary levels of prostanoids were determined in a group of six volunteers before and after intake of the thromboxane synthase inhibitor Ridogrel, and related to creatinine clearance.
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页码：599 / 611
页数：13
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