Simultaneous Determination of Aristolochic Acids Ⅰ and Ⅱ in Tongdi Capsules by UPLC-MS/MS
Objective:To establish an ultra-high performance liquid chromatography-mass spectrometry(UPLC-MS/MS)method for the determination of aristolochic acids Ⅰ and aristolochic acids Ⅱ in Tongdi Capsules.Methods:A Shiseido Shim-pack velox C18 chromatographic column(100 mm×2.1 mm,1.8 μm)was used with a gradient elution of acetonitrile(A)and 0.1%formic acid(with ammonium formate,B)as the mobile phase at a flow rate of 0.3 mL·min-1.Multiple reaction monitoring(MRM)was employed with aristolochic acid Ⅰ monitored at m/z 358.9→298.0(quantitative)and m/z 358.9→296.0(qualitative),and aristolochic acid Ⅱ at m/z 329.0→268.0(quantitative)and m/z 329.0→294.0(qualitative).The UPLC-MS method was established for the detection of aristolochic acids Ⅰ and aristolochic acids Ⅱ and applied to sample analysis.Results:Aristolochic acidⅠand aristolochic acid Ⅱshowed good linearity of injection volume with peak area at 1.052 4-420.960 0 pg and 1.002-100.200 ng,respectively(r>0.999).The spiked recovery rates were 97.63%and 92.34%with RSDs of 2.24%and 1.49%,respectively.In 15 batches of samples,the mass fractions of aristolochic acid Ⅰ and aristolochic acid Ⅱ ranged from 3.760 to 20.790 μg·g-1 and 0.010 to 0.156 μg·g-1,respectively.Conclusion:This method is sensitive,rapid,accurate,and highly specific,making it suitable for determining the content of aristolochic acid Ⅰ and aristolochic acid Ⅱ in Tongdi Capsules,which can provide a reference for medication safety.
万方数据
维普
