Journal of Lipid Research, Vol 18, 118-122, Copyright © 1977 by Lipid Research, Inc.
A facile hydrolysis-solvolysis procedure for conjugated bile acid sulfates
GP van Berge-Henegouwen, RN Allan, AF Hofmann and PY Yu
Methods for hydrolyzing and solvolyzing conjugated bile acid sulfates were
compared on reference mixtures of conjugated and unconjugated bile acid
sulfates 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 shich 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
1-hour incubation.