Simultaneous Determination of Pyrrolizidine Alkaloids and Aristolochic Acids in Fufang Banxia Tablets by UPLC-MS/MS and Risk Assessment
OBJECTIVE To establish an ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for simultaneous determination of three pyrrolizidine alkaloids and five aristolochic acids in Fufang Banxia Tablets,and carry out preliminary risk assessment.METHODS ACQUITY UPLC BEH C18 column(2.1 mm × 100 mm,1.7 μm)was used.The mixed solution of methanol-acetonitrile(1∶1)was used as mobile phase A,and 0.1%formic acid solution and 5 mmol·L-1 ammonium formate were used as mobile phase B.Gradient elution was performed at a flow rate of 0.3 mL·min-1 and the column temperature was maintainedat 30 ℃.Electrospray ion source(ESI),multiple reaction monitoring mode(MRM)and positive ion scan-ning were used.RESULTS Three pyrrolizidine alkaloids showed a good linear relationship in the range of 0.48-482.60 pg,and five aristolochic acids showed a good linear relationship in the range of 0.51-538.51 pg.The correlation coefficients were higher than 0.99.The average recoveries were between 60.4%%and 120.5%,with RSDs of 2.1%-9.7%.Pyrrolizidine alkaloids and aristolo-chic acids were detected in all five batches,the total content of pyrrolizidine alkaloids was 5.42-5.46 mg·kg-1,and the total con-tent of aristolochic acids in positive samples were 1.04-1.70 mg·kg-1.CONCLUSION The established method is simple and ac-curate,and can simultaneously determine the contents of three pyrrolizidine alkaloids and five aristolochic acids in Fufang Banxia Tablets.The preliminary risk assessment shows that the safety risk of Fufang Banxia Tablets is low.