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使用硅烷化试剂通过气相色谱法和气相色谱 - 质谱法鉴定羟基化甾体。酚羟基和醇羟基之间的区分。

Use of silylating agents for the identification of hydroxylated steroids by gas chromatography and gas chromatography-mass spectrometry. Discrimination between phenolic and alcoholic hydroxyl groups.

作者信息

Miyazaki H, Ishibashi M, Itoh M, Yamashita K, Nambara T

出版信息

J Chromatogr. 1977 Mar 21;133(2):311-8. doi: 10.1016/s0021-9673(00)83488-3.

DOI:10.1016/s0021-9673(00)83488-3
PMID:838812
Abstract

A phenolic trimethylsilyl (TMS) group was selectively exchanged for a dimethylalkylsilyl (DMAS) group on a gas chromatographic column by use of sandwich injection technique with DMAS-imidazole, and a TMS ether derivative of a phenolic steroid was converted into a DMAS ether or a mixed TMS and DMAS ether derivative with over 95% recovery. The selective exchange reaction seemed to be caused by the difference in lability between the ethereal TMS linkages to phenolic and alcoholic hydroxyl groups. This selectivity was found to be useful for discriminating gas chromatographically between the phenolic and alcoholic hydroxyl groups in steroids.

摘要

通过使用带有二甲基烷基硅烷基(DMAS)-咪唑的夹心进样技术,在气相色谱柱上酚羟基的三甲基硅烷基(TMS)基团被选择性地交换为二甲基烷基硅烷基(DMAS)基团,并且酚类甾体的TMS醚衍生物被转化为DMAS醚或TMS和DMAS混合醚衍生物,回收率超过95%。选择性交换反应似乎是由酚羟基和醇羟基的醚键合TMS的稳定性差异引起的。发现这种选择性可用于通过气相色谱法区分甾体中的酚羟基和醇羟基。

相似文献

1
Use of silylating agents for the identification of hydroxylated steroids by gas chromatography and gas chromatography-mass spectrometry. Discrimination between phenolic and alcoholic hydroxyl groups.使用硅烷化试剂通过气相色谱法和气相色谱 - 质谱法鉴定羟基化甾体。酚羟基和醇羟基之间的区分。
J Chromatogr. 1977 Mar 21;133(2):311-8. doi: 10.1016/s0021-9673(00)83488-3.
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