Determination of Gentiopicroside in Yaoxitong Capsules by UPLC-MS/MS
Objective To establish an ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for determining the content of gentiopicroside in Yaoxitong Capsules.Methods The UPLC chromatographic conditions were as follows:the chromatographic column was the Waters ACQUITY UPLC® BEH C18 column(100 mm×2.1 mm,1.7 μm),the mobile phase was 0.1%formic acid solution(containing 5 mmol/L ammonium acetate)-acetonitrile(gradient elution),the flow rate was 0.3 mL/min,the column temperature was 35℃,and the injection volume was 5 μL.The mass spectrometry conditions were as follows:the ion pair at the m/z 401.0 → 179.0 was the characteristic ion pair,the electrospray ion source(ESI)was adopted with negative ion scanning and multiple reaction monitoring(MRM)mode.Results The linear range of gentiopicroside was 0.055 1-22.022 3 μg/mL,the limit of detection was 6.7 ng/mL.The RSDs of precision,stability and repeatability tests were all lower than 2.1%.The content of gentiopicroside in 60 batches of samples was in the range of 27.66-3 367.24 μg/g,and that was significantly different among various manufacturing enterprises.Conclusion This method is easy,accurate,precise and repeatable,which can be used for the quality control of Yaoxitong Capsules.
万方数据
维普
