UHPLC-MS同时测定蛇胆川贝液中9种胆酸类成分

Simultaneous Determination of Nine Bile Acid Components in Shedan Chuanbei Liquid by UHPLC-MS

关键词:  蛇胆川贝液  胆酸类成分  超高效液相色谱-串联质谱法

Key words:  Shedan Chuanbei liquid  bile acid components  UHPLC-MS

摘要:

目的 采用UHPLC-MS同时测定蛇胆川贝液中9种胆酸类成分，分析不同企业、不同批次产品中胆酸类成分的差异。方法 采用Thermo Fisher Scientfic Bremen HYPERSIL GOLD(2.1 mm×100 mm，1.9 μm)为色谱柱，流动相为0.1%甲酸水溶液-甲醇，梯度洗脱，流速0.2 mL·min^-1，柱温为40 ℃。加热电喷雾离子源(HESI)负离子模式，质谱测定数据采用PRM扫描模式。结果 9种成分在各自范围内线性关系良好(r≥0.999 2)，平均加样回收率(95.5±1.52)%~(103.1±3.81)%，RSD 1.1%~5.5%。从19批供试品中共测得牛磺胆酸、牛磺熊去氧胆酸、7-酮-3α,12-α-羟基胆烷酸、牛磺鹅去氧胆酸、牛磺脱氧胆酸钠、胆酸、牛磺石胆酸钠、鹅去氧胆酸、去氧胆酸9种胆酸类成分；其中，牛磺胆酸、牛磺鹅去氧胆酸、牛磺脱氧胆酸钠3种胆酸类化合物在所有批次供试品中均可测出。结论 该方法简便稳定，对完善蛇胆川贝液的质量控制和评价方法具有一定参考价值。

Abstract:

OBJECTIVE To establish an UHPLC-MS method for simultaneous determination of 9 bile acids components in Shedan Chuanbei liquid. To analyze the differences of bile acids components from different manufacturers and different batches of product. METHODS Thermo Fisher Scientfic Bremen HYPERSIL GOLD(2.1 mm×100 mm, 1.9 μm) was selected as the chromatographic column. The mobile phase was 0.1% formic acid-water and methanol with gradient elution at a flow rate of 0.2 mL·min^-1, and the column temperature was 40 ℃. HESI negative ion mode was used for mass spectrometry, and PRM scanning mode was used for mass spectrometry data. RESULTS The calibration curves of 9 biles acids were linear in their own range(r≥0.999 2). The average recoveries ranged from (95.5±1.52)% to (103.1±3.81)%. The RSD ranged from 1.1% to 5.5%. Nine bile acids components including taurocholic acid, tauroursodesoxycholic acid, 7-ketone-3α,12-α-hydroxyl cholanic acid, taurochenodeoxy-cholic acid, sodium taurodeoxycholate, cholic acid, sodium taurocholate, chenodeoxycholic acid and deoxycholic acid were tentatively identified from 19 batches of test samples. Taurocholic acid, taurochenodeoxycholic acid and taurodeoxycholate sodium were detected in all the test batches. CONCLUSION This method is simple and stable, and has certain reference value for improving the quality control and evaluation of Shedan Chuanbei liquid.