HPLC-MS法同时测定钩藤药材中四种生物碱含量

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。

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

Objective:To establish the content determination method of four kinds of alkaloids in uncaria by HPLC-MS.Methods:Chromatographic conditions were as follows:HaloC_(18) 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-acetonitrile,gradient elution,the flow rate was 0.3 mL·min~(-1),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 were355.5 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.