Fischer S, Scherer B, Weber P C
Biochim Biophys Acta. 1982 Mar 12;710(3):493-501. doi: 10.1016/0005-2760(82)90134-5.
Endogenous levels of two metabolites of prostacyclin, 6-keto-prostaglandin F1 alpha (spontaneous hydrolysis product) and 6,15-diketo-13,14-dihydroprostaglandin F1 alpha (enzymatic degradation product) were measured in urine of adults and neonates by gas chromatography-mass spectrometry, using deuterated internal standards. The method comprised extraction of prostanoids by reverse-phase cartridges and purification by silicic acid column chromatography and reverse-and straight -phase high-performance liquid chromatographies. Exogenous 6-keto-prostaglandin F1 alpha and 6,15-diketo-13,14-dihydroprostaglandin F1 alpha added to urine were recovered quantitatively by gas chromatography-mass spectrometry. Endogenous levels of 6-keto-prostaglandin F1 alpha in urine of adults were 0.11 +/- 0.05 (S.D.) ng/ml (n = 12), whereas in urine of neonates the levels were much higher: 1.41 +/- 0.36 (S.D.) ng/ml (n = 5) on the 3rd day of life declining to 0.51 +/- 0.21 (S.D.) ng/ml (n = 5) on the 5th day. 6-keto-prostaglandin F1 alpha was also estimated in both age groups by radioimmunoassay. Urinary levels of 6,15-diketo-13, 14-dihydroprostaglandin F1 alpha in neonates on the 3rd day of life were 2.12 +/- 0.70 (S.D.) ng/ml (n = 4) and declined until the 5th day. In adult urine this metabolite was below the limit of detection (0.20 ng/ml).
采用气相色谱 - 质谱联用技术，以氘代内标物测定了成人和新生儿尿液中前列环素的两种代谢物——6 - 酮 - 前列腺素F1α（自发水解产物）和6,15 - 二酮 - 13,14 - 二氢前列腺素F1α（酶促降解产物）的内源性水平。该方法包括通过反相柱提取前列腺素类物质，并通过硅酸柱色谱以及反相和正相高效液相色谱进行纯化。气相色谱 - 质谱联用法定量回收了添加到尿液中的外源性6 - 酮 - 前列腺素F1α和6,15 - 二酮 - 13,14 - 二氢前列腺素F1α。成人尿液中6 - 酮 - 前列腺素F1α的内源性水平为0.11±0.05（标准差）ng/ml（n = 12），而新生儿尿液中的水平要高得多：出生第3天为1.41±0.36（标准差）ng/ml（n = 5），到第5天降至0.51±0.21（标准差）ng/ml（n = 5）。两个年龄组的6 - 酮 - 前列腺素F1α水平也通过放射免疫测定法进行了估算。新生儿出生第3天尿液中6,15 - 二酮 - 13,14 - 二氢前列腺素F1α的水平为2.12±0.70（标准差）ng/ml（n = 4），并持续下降至第5天。在成人尿液中，这种代谢物低于检测限（0.20 ng/ml）。
