UPLC-Q-Exactive-Orbitrap-MS法同时测定牛黄上清片中18种胆汁酸的含量OA北大核心CSTPCD

AIM To establish a ultra performance liquid chromatography-quadrupole-exactive orbitrap mass spectrometry(UPLC-Q-Exactive-Orbitrap-MS)method for the simultaneous content determination of taurocholic acid,7-ketodeoxycholic acid,glycohyodeoxycholic acid,12-oxochenodeoxycholic acid,gycocholic acid,3-oxo-7α,12α-hydroxy-5β-cholanoic acid,taurochenodeoxycholic acid,3-oxocholic acid,hyocholic acid,taurodeoxycholic acid sodium salt hydrate,hyodeoxycholic acid,cholic acid,gycochenodeoxycholic acid,glycodesoxycholic acid,taurolithocholic acid sodium salt,ghenodeoxycholic acid,deoxycholic acid and lthocolic acid in Niuhuang Shangqing Tablets.Then chemical pattern recognition was performed.METHODS The analysis was performed on a 40℃thermostatic Thermo Fisher Scientfic Bremen HYPERSIL GOLD column(2.1 mm×100 mm,1.9 μm),with the mobile phase comprising of 0.1%formic acid-methanol flowing at 0.2 mL/min in a gradient elution manner,and heating electron spray ionization source was adopted in negative ion scanning with parallel reaction monitoring mode.RESULTS Eighteen bile acids showed good linear relationships within their own ranges(r≥0.999 5),whose average recoveries were 96.73%-104.07%with the RSDs of 2.10%-4.07%.Certain differences in kind and content of bile acids in samples from different manufacturers were observable.CONCLUSION This sensitive,reliable and specific method can be used for the quality control of Niuhuang Shangqing Tablets.