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通过高效液相色谱法和直接化学电离质谱法鉴定前列腺素经重铬酸吡啶鎓衍生化后的反应产物。

Identification of reaction products from the pyridinium dichromate derivatization of prostaglandins by high-performance liquid chromatography and direct chemical ionization mass spectrometry.

作者信息

Doehl J, Greibrokk T

机构信息

Department of Chemistry, University of Oslo, Norway.

出版信息

J Chromatogr. 1989 Aug 30;477(2):345-57. doi: 10.1016/s0021-9673(01)89643-6.

DOI:10.1016/s0021-9673(01)89643-6
PMID:2808585
Abstract

The reaction products from the oxidation of prostaglandins with pyridinium dichromate have been identified by direct chemical ionization mass spectrometry of the underivatized compounds after separation by reversed-phase high-performance liquid chromatography and ultraviolet diode-array detection. The thermal influence on the reproducibility of the dehydration patterns of the mass spectra was studied. The main products from the prostaglandins E1, E2, F1 alpha and F2 alpha were the corresponding 15-oxo derivatives. Minor amounts of the 9,11,15-trioxoprostaglandin were formed from PGE, while the oxidation of PGF was less selective, yielding additional dioxo derivatives. Addition of water to the reagent reduced the reactivity, but increased the selectivity in favour of the formation of 15-oxo-PGF during the oxidation of PGF.

摘要

通过反相高效液相色谱分离和紫外二极管阵列检测后,对未衍生化的化合物进行直接化学电离质谱分析,已鉴定出前列腺素与重铬酸吡啶鎓氧化反应的产物。研究了热对质谱脱水模式重现性的影响。前列腺素E1、E2、F1α和F2α的主要产物是相应的15-氧代衍生物。PGE形成少量的9,11,15-三氧代前列腺素,而PGF的氧化选择性较低,产生额外的二氧代衍生物。向试剂中加水会降低反应活性,但在PGF氧化过程中会增加有利于形成15-氧代-PGF的选择性。

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