HPLC-MS法同时测定钩藤药材中四种生物碱含量

Content Determination of Four Kinds of Alkaloids in Uncaria by HPLC-MS

目的:建立钩藤药材中四种生物碱的高效液相色谱-质谱联用含量测定方法。方法:色谱条件:HaloC_(18)色谱柱(2.1 mm×100 mm,2.7μm),1%乙酸-水(氨水调pH=5.5)-甲醇-乙腈为流动相,梯度洗脱,流量0.3 mL·min^(-1),柱温35℃。质谱条件:电喷雾离子源,正离子检测方式,多反应监测模式,干燥气温度350℃,干燥气流量9 L·min^(-1),雾化器压力35 psi,毛细管电压4 000 V。结果:钩藤碱、异钩藤碱、去氢钩藤碱和异去氢钩藤碱含量分别为355.5μg·g^(-1)、143.9μg·g^(-1)、93.3μg·g^(-1)、202.7μg·g^(-1)。结论:该方法结果准确,重现性好,可用于测定钩藤药材中的生物碱含量。

Objective：To establish the content determination method of four kinds of alkaloids in uncaria by HPLC-MS. Methods ： Chromatographic conditions were as follows ： Halo C18 column （2.1 mm × 100 mm, 2.7 μm）, the mobile phase was a mixture of 1% acetic acid solution（adjusted pH=5.5 by ammonia）-methanol-acetoni- trile,gradient elution,the flow rate was 0.3 mL.min-l,the column temperature was 35 ℃. MS conditions：ESI ion source,detection method with positive ions,mode by MRM,drying temperature was 350 ℃ ,the flow rate of drying gas was 9 L.min-1 , pressure of nebulizer was 35 psi,the voltage of capillary was 4 000 V. Results ：The contents of rhynchophylline,isorhynchophylline,corynoxeine and isocorynoxeine in the samples were 355.5 μg. g-1, 143.9 μg. g-1,93.3 μg. g-1,202.7 μg. g-1 respectively. Conclusion ：The methods were accurate and the reproducibility was good,which can be used for determination of alkaloids in uncaria.