LC—MS／MS测定乌头属中药中8个生物碱含量

目的：建立LC-MS／MS测定乌头属中药8种生物碱含量的方法。方法：以甲醇-水（水相含0．1％甲酸和2．5mM醋酸铵溶液）为流动相，C18柱分离，采用ESI（＋）源，MRM监测，对制川乌、制草乌、制附子药材饮片中的双酯型生物碱（乌头碱、新鸟头碱、次乌头碱），单酯型生物碱（苯甲酰乌头原碱、苯甲酰新乌头原碱、苯甲酰次乌头原碱），胺醇型生物碱（乌头原碱、新鸟头原碱）进行含量测定。结果：上述8种生物碱的线性关系良好，精密度、重复性的RSD都低于6％，加样回收率为95．77％-101．90％。结论：该方法简便、快速、精密度高、重复性好，可应用于乌头属中药的质量控制。

Determination of 8 Alkaloids in Aconitum Species by LC-MSIMS

Objective： To establish an LC-MS/MS method for the determination of 8 alkaloids in Aconitum Species. Methods： Alkaloids were separated on an Aglient CI8 column using methanol and water （ 0.1 % formic acid and 2.5 mM ammonium acetate） as mobile phase. MS determination was performed by Electrospray Ionization （ ESI ） in positive mode using Multiple Reaction Monitoring （ MRM ） mode. Relying on the above method, diterpenoid alkaloids （Aconitine, esaconitine, Hypaconitine ）, monoester type alkaloids （Benzoylaconine, Benzoylmesaconitine, Benzoylhypaconitine ） and amine alcohols alkaloids （ Aconitine, Mesaconitine） were determined. Result： All the 8 alkaloids showed good linearity, the RSD of the precision, repeatability tests were less than 60/0, and the average recoveries were in the range of 95.77%-101.90%. Conclusion： The method is simple, rapid, high-precision and repeatable, so it is proposed for the effective guarantee of safety and efficacy of Aconitum Species in clinical medicine.