A facile hydrolysis–solvolysis procedure for conjugated bile acid sulfates
1977; Elsevier BV; Volume: 18; Issue: 1 Linguagem: Inglês
10.1016/s0022-2275(20)41722-5
ISSN1539-7262
AutoresGerard P. van Berge-Henegouwen, R N Allan, Alan F. Hofmann, Paulina Y. S. Yu,
Tópico(s)Drug Transport and Resistance Mechanisms
ResumoMethods for hydrolyzing and solvolyzing conjugated bile acid sulfates were compared on reference mixtures of conjugated and unconjugated bile acid SUIfates using gas-liquid chromatography to assess recovery, and thin-layer chromatography and zonal scanning to define the products occurring after hydrolysis.Conventional methods in which solvolysis preceded vigorous alkaline saponification gave incomplete recoveries.However, essentially complete recovery of primary and secondary bile acid sulfates was obtained with a mild alkaline saponification procedure followed by acidification and extraction into ether, in which complete solvolysis was shown to occur within 12 hours.Based on these findings, we developed and validated a simple hydrolysis-solvolysis procedure; the method features mild alkaline hydrolysis, acidification to pH 1, and extraction with ether followed by a I-hour incubation.Supplementary key words: solvolysis .conjugated bile acids * lithocholic acid * sulfated bile acids Bile acids present in body fluids are often identified and quantitated by gas-liquid chromatography (GLC).Since bile acids are present in bile and serum as the N-acyl glycine or taurine conjugates, a hydrolysis procedure has been an essential first step in the sequence of reactions entailed in the conversion of bile acids to volatile derivatives.Commonly, this is achieved by saponification in strong alkali ( l ) , although enzymatic deconjugation with cholylglycine
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