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荧光和紫外吸收胆汁盐衍生物的反相高效液相色谱法分离与形成

Formation and separation by reversed-phase high-performance liquid chromatography of fluorescent and UV-absorbing bile salt derivatives.

作者信息

Reid A D, Baker P R

出版信息

J Chromatogr. 1983 Apr 29;260(1):115-21. doi: 10.1016/0021-9673(83)80013-2.

DOI:10.1016/0021-9673(83)80013-2
PMID:6863432
Abstract

A method is described for the production of bile salt derivatives via the substituent hydroxyl groups on the steroid nucleus that permits derivatization of taurine and glycine conjugates. The method involves the oxidation of the hydroxyl groups at C-3 alpha or C-7 alpha on the nucleus by the action of hydroxysteroid dehydrogenases. The keto bile salts produced are isolated and reacted with 2,4-dinitrophenylhydrazine or Dns-hydrazine to yield ultraviolet absorbing or fluorescent derivatives, respectively. The bile salt hydrazones were separated using a reversed-phase C18 radial compression cartridge with a methanol-phosphate buffer gradient elution. Although the 3-keto derivatives of chenodeoxycholic and deoxycholic acids were not resolved, the 7-keto Dns-hydrazone of chenodeoxycholic acid was separated from 3-keto derivative of deoxycholic acid.

摘要

描述了一种通过甾体核上的取代羟基生成胆汁盐衍生物的方法,该方法可实现牛磺酸和甘氨酸共轭物的衍生化。该方法包括通过羟基甾体脱氢酶的作用氧化核上C-3α或C-7α位的羟基。分离生成的酮胆汁盐,并使其分别与2,4-二硝基苯肼或丹磺酰肼反应,以产生分别具有紫外吸收或荧光的衍生物。使用反相C18径向压缩柱,以甲醇 - 磷酸盐缓冲液梯度洗脱分离胆汁盐腙。虽然鹅去氧胆酸和脱氧胆酸的3-酮衍生物没有分离,但鹅去氧胆酸的7-酮丹磺酰腙与脱氧胆酸的3-酮衍生物得以分离。

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Formation and separation by reversed-phase high-performance liquid chromatography of fluorescent and UV-absorbing bile salt derivatives.荧光和紫外吸收胆汁盐衍生物的反相高效液相色谱法分离与形成
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