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人尿和兔尿中前列腺素F2α的质量碎片分析法测定

Mass fragmentographic determination of prostaglandin F2 alpha in human and rabbit urine.

作者信息

Sjöquist B, Oliw E, Lundén I, Anggård E

出版信息

J Chromatogr. 1979 May 1;163(1):1-9. doi: 10.1016/s0378-4347(00)81162-7.

Abstract

Analysis of prostaglandin F2 alpha (PGF2 alpha) in urine is a useful indicator of renal prostaglandin synthesis. A mass fragmentographic method for PGF2 alpha analysis in human urine was developed using [3,3,4,4-2H4]PGF2 alpha as an internal standard and carrier. PGF2 alpha was extracted from urine (20 ml) with chloroform, purified by preparative thin-layer chromatography and converted to the methyl ester trimethylsilyl ether before analysis by gas chromatography--mass spectrometry. The specificity of the urine analysis was demonstrated by retention time and the use of two pairs of fragments m/e 494/498 and 513/517 with the same results. The coefficient of variation for duplicate analysis averaged 12.6%, n = 17. Urine from recumbent women contained 4.9 +/- 2.6 (S.D.) ng/ml or 4.1 +/- 1.0 ng PGF2 alpha per mg creatinine (n = 10) with little diurnal variation. Male urine contained 5.0 +/- 2.7 (S.D.) ng/ml or 3.7 +/- 2.1 ng/mg creatinine (n = 10). Similar concentrations were found in boys and in girls. These observations indicate that urinary PGF2 alpha originates from the kidneys with little contribution from the male accessory sexual glands. This method can also be applied to analysis of PGF2 alpha in rabbit urine.

摘要

尿液中前列腺素F2α(PGF2α)的分析是肾前列腺素合成的一项有用指标。利用[3,3,4,4-2H4]PGF2α作为内标和载体,开发了一种用于分析人尿液中PGF2α的质量碎片分析法。PGF2α从20毫升尿液中用氯仿提取,通过制备性薄层色谱法纯化,并在通过气相色谱-质谱分析之前转化为甲酯三甲基硅醚。通过保留时间以及使用两对m/e 494/498和513/517的碎片且结果相同,证明了尿液分析的特异性。重复分析的变异系数平均为12.6%,n = 17。卧位女性尿液中PGF2α含量为4.9±2.6(标准差)纳克/毫升或每毫克肌酐4.1±1.0纳克PGF2α(n = 10),昼夜变化很小。男性尿液中含量为5.0±2.7(标准差)纳克/毫升或3.7±2.1纳克/毫克肌酐(n = 10)。男孩和女孩中发现了类似的浓度。这些观察结果表明,尿中PGF2α源自肾脏,男性附属性腺的贡献很小。该方法也可应用于兔尿液中PGF2α的分析。

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