Adulteration of Bupleurum marginatum var.stenophyllum in Gengnianning water-honeyed pill by UPLC-MS/MS
Objective To establish the detection method for the adulteration of Bupleurum marginatum var.stenophyllum in Gengnianning water-honeyed pill,and to find out whether Bupleurum marginatum var.stenophyllum was used to replace Bupleuri Radix in the manufacturing enterprises.Methods UPLC-MS/MS was performed on Waters BEH C18 column(2.1 mm×50 mm,1.7 μm),with acetonitrile and 0.1％formic acid as the mobile phase in gradient elution at 0.3 mL·min-1.The column temperature was 35 ℃ and the injection volume was 1 µL.A triple quadrupole mass spectrometer was used for the detection in negative ion mode with an electrospray ion source.m/z 943.5 → 635.4,m/z 943.5 → 797.5 and m/z 943.5 → 781.5 were selected as the ion pairs and multiple reaction monitoring(MRM)mode was used for the determination of nepasaikosaponin K.Results Nepasaikosaponin K showed a good linearity at 93.3～3734 ng·mL-1(r=0.9998).The RSDs of precision,repeatability and stability(24 h)were all lower than 2.0％.The average recoveries at three spiked levels were 96.4％～99.6％(RSD＜3.0％).The adulteration ratio of Bupleurum marginatum var.stenophyllum in Gengnianning water-honeyed pill showed a good linearity to the content of nepasaikosaponin K within 3％～100％(r=0.9947).Totally 44 batches of Gengnianning water-honeyed pill were screened with the limit that the doping of Bupleurum marginatum var.stenophyllum should not exceeding 10％.The doping of Bupleurum marginatum var.stenophyllum in 5 batches of Gengnianning water-honeyed pill was 22％～36％,which exceeded the proposed limit.Conclusion The method is accurate and reliable,can be used to detect the adulteration of Bupleurum marginatum var.stenophyllum in Gengnianning water-honeyed pill.
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