HPLC-Q-TOF-MS法测定不同厂家小金丸中9种乌头类生物碱的含量

摘要

ABSTRACT:OBJECTIVE To establish an HPLC-Q-TOF-MS method for the determination of 9 Aconitum alka-loids(Aconitine,Hypaconitine,Mesaconitine,Benzoylaconine,Benzoylhypaconine,Benzoylmesaconine,Aconine,Hyp-aconine,Mesaconine) in Xiaojin pills from different factories.METHODS Column:ZORBAX Extend-C18 RRHT (1.8μm,2.1 ×50mm);flow rate was 0.21mL· min -1;the column temperature was 30℃;the mobile phase consis-ted of methanol-water(containing 0.1% formic acid and 2.5mmol· L-1 ammonium acetate) using a gradient pro-gramme;Ion source:ESI+;RESULTS All the 9 alkaloids showed good linearity(r>0.9997),the RSD of the pre-cision,repeatability and stability tests were less than 5%.The average recoveries were in the range of 98.73%~103.54%.CONCLUSION The method is simple,rapid,sensitive,high-precision and repeatable.So it is proposed for the effective guarantee of safety and efficacy of Xaiojin Pills.%目的：建立高效液相色谱-四级杆飞行时间串联质谱（ HPLC-Q-TOF-MS）法测定不同厂家小金丸中乌头类生物碱（乌头碱、次乌头碱、新乌头碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰新乌头原碱、乌头原碱、次乌头原碱、新乌头原碱）的含量。方法色谱柱：ZORBAX Extend-C18 RRHT柱（1.8μm，2.1×50mm）；流速为0.21mL· min -1；柱温：30℃；流动相：甲醇-水（水相含0.1%甲酸和2.5mmol· L -1醋酸铵溶液）系统梯度洗脱；采用电喷雾离子（ESI）源，正离子方式检测。结果上述9种生物碱在一定范围内具有较好的线性关系，r值均大于0.9997，精密度、重复性和稳定性的RSD都低于5%，加样回收率均在98.73%~103.54%之间。结论该方法简便、快速、灵敏、精密度高、重复性好，可应用于小金丸的质量控制。