SPE-HPLC测定复方羊角颗粒中苯甲酰新乌头原碱等3个单酯型生物碱的含量

Determination of Three Monoester Aconitum Alkaloids Including Benzoylmesaconitine in Compound Yangjiao Granules by SPE-HPLC

目的:建立复方羊角颗粒中苯甲酰新乌头原碱等3个单酯型生物碱的含量测定方法。方法:采用强阳离子吸附树脂MCX固相萃取小柱对复方羊角颗粒进行净化,高效液相色谱法测定,色谱柱:SVEA^(TM)C_(18)Opal(4.6 mm×250 mm,5μm);流动相A为乙腈-四氢呋喃(25∶12),流动相B为0.1 mol·L^(-1)醋酸铵溶液(含0.05%冰醋酸),梯度洗脱;检测波长:235 nm;柱温:25℃;流速:1.0mL·min^(-1);进样量:20μL。结果:苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱的线性范围分别为2.27~98.61(r=1.0000)、0.61~26.53(r=1.0000)、1.00~43.50μg·m L^(-1)(r=0.999 9);平均回收率及RSD分别为93.9%及2.4%、95.0%及2.6%、91.0%及3.0%。结论:本方法可为复方羊角颗粒的质量控制提供依据。

Objective:To establish a method for the determination of benzoylmesaconitine,benzoylhypaconitine and benzoylaconitine in compound Yangjiao granules.Methods:The compound Yangjiao granules were purified by solid-phase extraction using a strong cationic adsorption resin MCX column.HPLC was used for determination with a SVEA^(TM)C_(18)Opal (4.6 mm×250 mm,5μm) column.Acetonitrile-THF (25∶12(A)-0.1 mol·L^(-1))ammonium acetate solution (containing 0.05%acetic acid)(B) as the mobile phase was applied for gradient elution at a flow rate of 1.0 mL·min^(-1).The detection wavelength was 235 nm and the column temperature was 25°C.The injection volume was 20μL.Results:The linear ranges of benzoylmesaconitine,benzoylhypaconitine and benzoylaconitine were 2.27-98.61 (r=1.000 0),0.61-26.53 (r=1.000 0and 1.00-43.50μg·mL^(-1)(r=0.999 9)),respectively.The average recovery rates of the above compounds were 93.9%,95.0%and 91.0%with RSD of 2.4%,2.7%and 3.0%,respectively.Conclusion:The proposed method offered a reference for quality control of compound Yangjiao granules.