HPLC法同时测定风湿骨痛片中12个乌头碱类成分的含量  

Determination of 12 aconite alkaloids in Fengshi Gutong tablets by HPLC

作　　者：卢虹妃 倪倩 冯有龙 LU Hong-fei;NI Qian;FENG You-long(China Pharmaceutical University,Nanjing 211198,China;Jiangsu Institute for Food and Drug Control,Nanjing 210019,China)

机构地区：[1]中国药科大学,南京211198 [2]江苏省食品药品监督检验研究院,南京210019

出　　处：《药物分析杂志》2024年第9期1578-1585,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：江苏省市场监督管理局科研计划项目(KJ204121)。

摘　　要：目的:建立风湿骨痛片中乌头碱类成分的含量测定方法。方法:采用Waters XSelect■CSH C_(18)色谱柱(250 mm×4.6 mm,5μm),以0.1%醋酸水溶液-乙腈-甲醇系统为流动相进行梯度洗脱,流速1.0 mL·min^(-1),检测波长245 nm,柱温30℃。结果:冉乌头碱、苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、8-去乙酰基滇乌碱、10-羟基新乌头碱、新乌头碱、次乌头碱、印乌头碱、乌头碱、滇乌头碱、草乌甲素的进样量分别在0.0228~0.1366μg、0.0415~0.2490μg、0.0335~0.2008μg、0.0339~0.2031μg、0.0331~0.1986μg、0.0403~0.2416μg、0.0302~0.1814μg、0.0286~0.1716μg、0.0336~0.2016μg、0.0303~0.1819μg、0.0634~0.3815μg、0.0340~0.2042μg时,其峰面积与进样量呈现良好的线性关系;精密度、重复性、稳定性试验结果均满足有关技术要求;上述12个乌头碱类成分的平均回收率分别在93.6%~101.5%,RSD分别在0.55%~3.3%。3批风湿骨痛片(批号211227、220823、230425)中冉乌头碱、苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、8-去乙酰基滇乌碱、10-羟基新乌头碱、新乌头碱、次乌头碱、印乌头碱、滇乌头碱的每片平均含量为0.492、65.78、7.319、10.164、1.068、5.583、2.573、5.865、2.021、2.050μg;乌头碱、草乌甲素未检出。结论:所建立的方法专属性强、灵敏度和准确度均较高,可用于风湿骨痛片中12个乌头碱类成分的含量测定,实现对制剂进行全面的质量控制。Objective:To establish a method for determination of aconite alkaloids in Fengshi Gutong tablets.Methods:Analysis was performed on a WatersXSelect■CSH C_(18)(250 nm×4.6 mm,5μm)column with mobile phase consisting of 0.1%acetic acid aqueous solution,acetonitrile and methanol with gradient elution at a flow rate of 1.0 mL·min^(-1).The detection wavelength was set at 245nm and the column temperature was 30℃.Results:Twelve aconite alkaloids could be separated well.When the injection amounts of ranaconitine,benzoylmesaconine,benzoylmesaconine,benzoylmesaconine,acoforestinine and beiwutine,mesaconitine,hypaconitine,indaconitine,aconitine,yunaconitine,bulleyaconitine A were 0.0228-0.1366μg,0.0415-0.2490μg,0.0335-0.2008μg,0.0339-0.2031μg,0.0331-0.1986μg,0.0403-0.2416μg,0.0302-0.1814μg,0.0286-0.1716μg,0.0336-0.2016μg,0.0303-0.1819μg,0.0634-0.3815μg and 0.0340-0.2042μg,respectively,the peak area showed a good linear relationship with the injection amounts.The average recovery rates of 12 aconite alkaloid components ranged from 93.6%to 101.5%,and the RSD ranged from 0.55%to 2.6%.The average contents of ranaconitine,benzoylmesaconine,benzoylmesaconine,benzoylmesaconine,acoforestinine and beiwutine,mesaconitine,hypaconitine,indaconitine and yunaconitine in three batches of Fengshi Gutong tablets(batch No.211227,220823 and 230425)were 0.492μg,65.78μg,7.319μg,10.164μg,1.068μg,5.583μg,2.573μg,5.865μg,2.021μg,2.050μg,respectively.And aconitine and bulleyaconitine A were not detected.Conclusions:The established method is accurate and reliable,and can be used for the determination of 12 aconite alkaloids compounds in Fengshi Gutong tablets to achieve comprehensive quality control of preparations.

关 键 词：风湿骨痛片 乌头碱 草乌甲素 高效液相色谱 质量控制 

分 类 号：R917[医药卫生—药物分析学]