RESUMEN
An ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q Exactive-Orbitrap MS) method for the simultaneous determination of 15 compounds (taurocholic acid, 7-keto-3α,12-α-dihydroxycholanic acid, glycocholic acid, 3-oxo-7α,12α-hydroxy-5β-cholanoic acid, taurochenodeoxycholic acid, 3α-hydroxy-7-oxo-5β-cholanic acid, hyocholic acid, sodium taurodeoxycholate, hyodeoxycholic acid, cholic acid, glycochenodeoxycholic acid, glycodeoxycholic acid, taurolithocholic acid sodium salt, chenodeoxycholic acid, deoxycholic acid) in Niuhuang Jiangya Pills was established. The separation was performed on a Thermo Fisher Scientfic Bremen HYPERSIL GOLD C18 column (100 mm × 2.1 mm, 1.9 μm). Methanol and water (containing 0.1% formic acid)were adopted as the mobile phase by gradient elution．MS detection was performed with multiple reaction monitoring mode．The results showed that fifteen compounds had a good linearity within their respective concentration ranges (r > 0.999 0). The average recovery rates were 93.7%- 105.2% (n = 9). The established method was used to determine the content of 15 batches of samples, and the results showed that the content of cholic acid was quite different. The present study provides an important reference for the overall quality control of Niuhuang Jiangya Pills.
RESUMEN
AIM To establish a ultra-high performance liquid chromatography coupled with triple quadruple mass spectrometry (UPLC-QQQ-MS) method for the simultaneous content determination of notoginsenoside R1,ginsenoside Re,ginsenoside Rg1,ginsenoside Rb1,ginsenoside Rd,taurine,taurocholic acid,cholic acid,glycocholic acid,glycodeoxycholicacid,chenodeoxycholic acid,deoxycholic acid and muscone in Pientzehuang (Bovis Calculus,Moschus,Notoginseng Radix et Rhizoma,etc.).METHODS The analysis of methanol extract of this drug was performed on a 40 ℃ thermostatic Waters CORTECS UPLC C18column (100 mm × 2.1 mm,1.6 μm),with the mobile phase comprising of acetonitrile-water (containing 0.1％ formic acid) flowing at 0.25 mL/min in a gradient elution manner.RESULTS Thirteen constituents showed good linear relationships within their own ranges (r ＞0.998 5),whose average recoveries were 91.1％-105.3％ with the RSDs of 2.4％-4.6％.CONCLUSION This accurate,simple,sensitive and reproducible method can be used for the quality control of Pientzehuang.