HPLC同时测定成药中4种乌头类生物碱含量

HPLC simultaneous determination of four aconitine alkaloids in patent medicine

目的:建立一种同时测定含有乌头属药材的成药中乌头类生物碱宋果灵、新乌头碱、乌头碱、次乌头碱含量的HPLC方法。方法:采用Kromasil C18色谱柱(4.6mm×250mm,5μm),以甲醇-水-氯仿-三乙胺(70:30:1:0.15)为流动相,流速1.0mL.min-1,柱温为室温(25℃),检测波长234nm。结果:宋果灵、新乌头碱、乌头碱和次乌头碱的线性范围分别为0.1～1.5μg(r=0.9996),0.1～2.0μg(r=0.9995),0.1～3.0μg(r=0.9996),0.1～2.5μg(r=0.9997)。本法应用于中成药万通筋骨片、附子理中丸,藏药安神丸和蒙药嘎日迪五味丸中4种乌头类生物碱的同时测定,宋果灵、新乌头碱、乌头碱和次乌头碱的平均回收率分别为95.7%～105.2%,96.0%～102.1%,93.7%～99.2%,96.8%～99.2%;RSD分别为1.4%～2.3%,1.0%～1.8%,0.85%～2.2%,0.82%～1.4%。结论:本法简便、快速、准确,灵敏度高,可为含有乌头属药材的成药药品质量控制提供参考标准。

Objective：To establish an HPLC method for simultaneous determination of aconitine alkaloids in patent medicine contained Aconitum L.herbal drugs.Method：The separation was performed on a Kromasil C18 column （4.6 mm×250 mm,5 μm） and methanol-water-chloroform-triethylamine （70∶30∶1∶0.15） as mobile phase with a flow rate of 1.0 mL·min-1.UV detection was set at 234 nm and column temperature was room temperature（25 ℃）.Results：The standard calibration curves of songorine,mesaconitine,aconitine and hypaconitine were linear in the ranges of 0.1-1.5 μg （r=0.9996）,0.1-2.0 μg （r=0.9995）,0.1-3.0 μg （r=0.9996） and 0.1-2.5 μg（r=0.9997）,respectively.This method was applied to simultaneous determination of four aconitine alkaloids in Wantongjingu tablets and Fuzilizhong pills as Chinese patent medicine;Anshen pills as Sitsang medicine and Garidiwuwei pills as Mongolia medicine.The average recoveries of method in the four patent medicines were 95.7%-105.2%,96.0%-102.1%,93.7%-99.2% and 96.8%-99.2%,and RSD were 1.4%-2.3%,1.0%-1.8%,0.85%-2.2% and 0.82%-1.4%,respectively.Conclusion：This method is simple,quick,accurate,and with high sensitivity.It provides a reference standard for the quality control of patent medicine contained Aconitum L.herbal drugs.