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 |
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引用本文: | 黄阳,曹益鸣,张小龙,卜红闽.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[J].海峡药学,2016(9):57-60. |
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作者姓名: | 黄阳 曹益鸣 张小龙 卜红闽 |
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作者单位: | 1. 昆山市中医医院 昆山 215300;2. 连云港市药品检验所 连云港222006 |
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摘 要: | 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。
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关 键 词: | HPLC-Q-TOF-MS 小金丸 乌头类生物碱 含量测定 |
Determination of Nine Aconitum Alkaloids in Xiaojin Pills from Different Factories by HPLC-Q-TOF-MS |
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Abstract: | 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. |
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Keywords: | HPLC-Q-TOF-MS Xiaojin pills Aconitum alkaloids Determination |
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