HPLC同时测定附子理中丸中3种单酯型生物碱含量  

Simultaneous Determination of Benzoylmesaconitine,Benzoylaconitine and Benzoylhypaconitine in Fuzi Lizhong Pills by HPLC

作　　者：邵峰[1] 俞瑜[1] 任刚[1] 黄慧莲[1] 刘荣华[1] 谷丽菲[1] 刘科兰[1] 

机构地区：[1]江西中医学院现代中药制剂教育部重点实验室,南昌330004

出　　处：《中国实验方剂学杂志》2012年第16期57-61,共5页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家自然科学基金项目(30801520);江西省教育厅项目(GJJ10212);江西省卫生厅项目(2010A029;2010A100)

摘　　要：目的:建立附子理中丸中3种单酯型生物碱(苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱)的含量测定方法。方法:色谱柱Alltimate C18(4.6 mm×250 mm,5μm);保护柱Alltimate C18(4.6 mm×7.5 mm,5μm);流动相40 mmol.L-1乙酸铵(加氨水调pH 10.00±0.5)-乙腈梯度洗脱;流速1.0 mL.min-1,检测波长240 nm,柱温35℃。结果:苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱分别在进样量0.212～1.272μg,0.011 6～0.069 6μg,1.035～6.210μg线性关系良好,r分别为0.999 6,0.999 7,0.999 6,在8 h内稳定性良好。同时,针对苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱,附子理中丸(河南宛西)平均加样回收率依次为97.59%(RSD 1.90%)、98.81%(RSD 2.00%)、98.37%(RSD 1.72%),附子理中丸(安徽东芝堂)平均加样回收率依次为98.18%(RSD 2.39%)、103.06%(RSD 1.77%)、98.23%(RSD 2.05%),而附子理中丸(北京同仁堂)仅含苯甲酰新乌头原碱的平均加样回收率100.17%(RSD 2.29%)。结论:方法结果准确可靠、快速,适用于构建附子理中丸成方制剂的多指标质量评价模式。Objective： To develope an HPLC method for simuhaneously determining benzoylmesaconitine, benzoylaconitine and benzoylhypaconitine in Fuzi Lizhong pills. Method： The Alltimate C18 column （4.6 mm× 250 mm, 5 μm） and Alhimate Clsguard column （7.5 mm×4.6 mm, 5μm） were used; the mobile phase consisting of acetonitrile-40 mmol·L^-1 ammonium acetate （adjusted by ammonia pH value at 10. 00± 0.5） by gradient elutiou; the flow rate was 1.0 mL·min^-1; the detection wavelength was set at 240 nm with column temperature at 35℃. Result： The good linear range of benzoylmesaconitine, benzoylaconitine and benzoylhypaconitine was 0. 212-1. 272 p.g （r =0. 999 6）, 0. 011 6-0. 069 6μg （r =0. 999 7） and 1. 035-6.210 μg （r =0. 999 6） , respectively, and their average recoveries were 97.59% , 98.81% and 98.37% , also with RSD of 1.90% , 2.00% , 1.72% （n = 6） , from Henan Wanxi pharmaceutical Co, respectively. Their average recoveries were 98. 18%, 103.66% and 98.23%, also with RSD of 2.39%, 1.77%, 2.05% （n=6）, from Anhui Dongzhitang pharmaceutical Co, respectively. The average recovery of benzoylmesaconitine was 100. 17%with RSD of 2.29% （n=6） benzoylaconitine and convenient, rapid and benzoy accurat from Beijing ypaconiti e, which Be Tongrentang pharmaceutical Co. The was good during 8 h, respectively stability of benzoylmesaconitine, Conclusion： The method is can be used for the quality control of Fuzi Lizhong pills.

关 键 词：附子理中丸 高效液相色谱 苯甲酰新乌头原碱 苯甲酰乌头原碱 苯甲酰次乌头原碱 

分 类 号：R284.1[医药卫生—中药学]