小活络丸中乌头类生物碱成分含量测定方法的建立  

Establishment of Content Determination Method of Aconitum Alkaloids in Xiaohuoluo Pills

作　　者：赵振霞 苏建 曹春琪 王璐 刘永利 Zhao Zhenxia;Su Jian;Cao Chunqi;Wang Lu;Liu Yongli(Hebei Institute for Drug and Medical Device Control,Heibei Key Laboratory of Traditional Chinese Medicine Quality Evaluation and Standard Research,Shijiazhuang 050227,China)

机构地区：[1]河北省药品医疗器械检验研究院,河北省中药质量评价与标准研究重点实验室,石家庄050227

出　　处：《中国药事》2023年第7期798-807,共10页Chinese Pharmaceutical Affairs

基　　金：河北省市场监督管理局科研计划项目川乌、附子及其制剂中毒性成分质量控制方法研究(编号2021YJ01)。

摘　　要：目的:建立小活络丸中生物碱成分乌头碱、次乌头碱、新乌头碱、苯甲酰乌头原碱、苯甲酰次乌头原碱与苯甲酰新乌头原碱的含量测定方法,以完善其质量标准。方法:采用高效液相色谱法,选择PICKERING C_(18)(4.6 mm×250 mm,5μm)色谱柱,以甲醇、乙腈和0.1%磷酸水为流动相,梯度洗脱,流速1.0 mL·min^(-)1,柱温25℃,检测波长232 nm,进样量15μL。结果:乌头碱、次乌头碱、新乌头碱、苯甲酰乌头原碱、苯甲酰次乌头原碱及苯甲酰新乌头原碱分别在各自范围内线性关系良好(r=0.9999),平均加样回收率分别为99.8%(RSD=0.8%)、99.9%(RSD=1.0%)、100.6%(RSD=1.4%)、100.8%(RSD=1.5%)、100.9%(RSD=1.5%)、100.6%(RSD=0.8%)。5批样品中上述6个成分含量范围分别为0.5~2.9、5.4~27.4、0.5~10.5、18.8~24.6、18.8~30.2及142.4~181.6μg·g^(-1)。结论:所建立的同时测定6个生物碱含量的测定方法可准确测定小活络丸中生物碱成分的含量,有助于提高小活络丸的质量标准。Objective:To establish the method for determination of aconitine,hypaconitine,mesaconitine,benzoylaconine,benzoylhypaconine and benzoylmesaconine in Xiaohuoluo Pills,in order to improve its quality standard.Methods:HPLC was performed on PICKERING C18 column(4.6 mm×250 mm,5μm)with mobile phases composed of methanol-acetonitrile-0.1%phosphoric acid solution at a fl ow rate of 1.0 mL·min^(-1)ingradient elution mode.The column temperature was 25℃,the detection wavelength was 232 nm and the injection volume was 15μL.Results:Aconitine,hypaconitine,mesaconitine,benzoylaconine,benzoyl hypaconine and benzoylmesaconine showed good linear relationships in their respective ranges(r>0.9999),average sample recoveries were 99.8%(RSD=0.8%),99.9%(RSD=1.0%),100.6%(RSD=1.4%),100.8%(RSD=1.5%),100.9%(RSD=1.5%),100.6%(RSD=0.8%)respectively.The content ranges of six ingredients in 5 batches of samples were 0.5-2.9,5.4-27.4,0.5^(-1)0.5,18.8-24.6,18.8-30.2 and 142.4^(-1)81.6μg·g^(-1),respectively.Conclusion:The established method for simultaneous determination of 6 alkaloids could accurately determine the content of aconitum alkaloids in Xiaohuoluo Pills,which is helpful to improve the quality standard of Xiaohuoluo Pills.

关 键 词：小活络丸 乌头碱 次乌头碱 新乌头碱 苯甲酰乌头原碱 苯甲酰次乌头原碱 苯甲酰新乌头原碱 含量测定 

分 类 号：R917[医药卫生—药物分析学]