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通过薄层色谱法和高效液相色谱法测定药品中的游离胆汁酸。

Determination of free bile acids in pharmaceuticals by thin layer chromatography and high performance liquid chromatography.

作者信息

Novaković J, Tvrzická E, Razić S

机构信息

PRO.MED.CS,Telcská 1, Prague, Czech Republic.

出版信息

Boll Chim Farm. 1998 Nov;137(10):412-6.

PMID:9880946
Abstract

High-performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD) and thin layer chromatography with flame ionization detection (TLC-FID) have been applied to the separation of five main free bile acids present in humans: cholic (CA), chenodeoxycholic (CDCA), deoxycholic (DCA), lithocholic (LCA) and ursodeoxycholic (UDCA) acid. HPLC separation was performed on Biospher Si 100 column using a mixture of n-heptane, isopropanol, ethylacetate, methanol and glacial acetic acid as a mobile phase. All the compounds were separated in less than 12 minutes by using a gradient elution mode. TLC-FID separation was performed on S-II Chromarods with a mixture of isooctane, ethylacetate and glacial acetic acid as a mobile phase. HPLC-ELSD method was applied to the determination of CDCA and UDCA in pharmaceuticals and their purity control when LCA, DCA and CA were considered as impurities.

摘要

高效液相色谱-蒸发光散射检测法(HPLC-ELSD)和薄层色谱-火焰离子化检测法(TLC-FID)已用于分离人体中存在的五种主要游离胆汁酸:胆酸(CA)、鹅去氧胆酸(CDCA)、脱氧胆酸(DCA)、石胆酸(LCA)和熊去氧胆酸(UDCA)。HPLC分离在Biospher Si 100柱上进行,使用正庚烷、异丙醇、乙酸乙酯、甲醇和冰醋酸的混合物作为流动相。通过梯度洗脱模式,所有化合物在不到12分钟内得以分离。TLC-FID分离在S-II型棒状薄层板上进行,使用异辛烷、乙酸乙酯和冰醋酸的混合物作为流动相。当将LCA、DCA和CA视为杂质时,HPLC-ELSD方法用于药物中CDCA和UDCA的测定及其纯度控制。

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