超高效液相色谱串联质谱法同时测定走川骨刺酊中3种乌头类生物碱含量

目的建立同时测定走川骨刺酊中3种乌头类生物碱含量的超高效液相色谱-串联质谱(UPLC-MS/MS)法。方法色谱柱为ACQUITY UPLCBEH C18柱(50 mm×2.1 mm,1.7μm),流动相为0.1%甲酸溶液-乙腈(梯度洗脱),流速为0.25 m L/min,柱温为35℃,进样量为10μL;采取电喷雾离子源(ESI),正离子模式,采集方式为多反应监测(MRM)。结果乌头碱、次乌头碱、新乌头碱质量浓度分别在0.9198~91.9800 ng/m L(r=0.9978,n=7),1.048~104.800 ng/m L(r=0.9974,n=7),1.268~126.800 ng/m L(r=0.9998,n=7)范围内与峰面积线性关系良好,加样回收率分别为104.22%,105.05%,104.34%,RSD分别为3.13%,1.63%,1.62%(n=6)。结论该方法操作简便,精密度、重复性好,专属性高,结果准确,可用于同时测定走川骨刺酊中3种乌头类生物碱的含量。

Content Determination of Three Kinds of Aconitine Alkaloids in the Zouchuan Guci Tincture by UPLC-MS/MS

Objective To establish an ultra-performance liquid chromatography(UPLC)-MS/MS method for the content determination of three kinds of aconitine alkaloids in the Zouchuan Guci Tincture.Methods The chromatographic column was ACQUITY UPLCBEH C18 column(50 mm×2.1 mm,1.7μm),the mobile phase was 0.1%formic acid solution-acetonitrile(gradient elution),the flow rate was 0.25 m L/min,the column temperature was 35℃,the injection volume was 10μL,the electrospray ionization source(ESI)was adopted with positive ion mode,and the collection mode was multi-response monitoring(MRM).Results The linear ranges of aconitine,hypaconitine and mesaconitine were 0.9198-91.9800 ng/m L(r=0.9978,n=7),1.048-104.800 ng/m L(r=0.9974,n=7)and 1.268-126.800 ng/m L(r=0.9998,n=7),respectively.The recoveries were 104.22%,105.05%and 104.34%,and the RSDs were 3.13%,1.63%,1.62%(n=6).Conclusion The method is simple,has good precision,repeatability,specificity and accuracy,and can be used for the simultaneous determination of aconitine alkaloids in Zouchuan Guci Tincture.