参附注射液中3种痕量成分乌头碱、次乌头碱、新乌头碱的测定  

Determination of aconitine,hypaconitine and mesaconitine in Shenfu injection

作　　者：张盼盼[1] 张俊贞[2] 王朝虹[3] 卢永江 蒋晔[1] 

机构地区：[1]河北医科大学药学院,河北石家庄050017 [2]河北医科大学第四医院,河北石家庄050011 [3]最高人民检察院司法鉴定中心,北京100040 [4]山东莒县中医院,山东日照276500

出　　处：《中国中药杂志》2013年第10期1521-1525,共5页China Journal of Chinese Materia Medica

摘　　要：该文建立了参附注射液中3种痕量附子指标成分的含量测定方法,为评价君药附子的药效学作用提供了依据。样品经中空纤维液相微萃取(HF-LPME)进行纯化富集,采用ACQUITY UPLC BEH C18色谱柱(2.1 mm×50 mm,1.7μm),流动相乙腈-10 mmol.L-1碳酸氢铵溶液(pH 10),流速0.45 mL.min-1,梯度洗脱。电喷雾电离(ESI)、多反应监测(MRM)方式进行含量测定。结果表明,乌头碱、次乌头碱、新乌头碱在0.1～100 ng.L-1线性关系良好,r>0.999,检测限分别为0.03,0.03,0.02 ng.L-1,平均加样回收率分别为100.1%,97.4%,97.5%,RSD分别为1.2%,1.1%,1.5%。该方法保证了参附注射液的用药安全,为正确评价附子的君药药效学作用提供了科学依据,为含有附子的中药制剂的质量控制提供了可靠方便而实用的检测手段。To establish a method for the content determination of indexes for measuring aconitic compounds contained in Shen- fu injection, in order to provide basis for the evaluation of the curative effect of monkshood in Shenfu injection. The sample were purified and enriched with HF-LPME. ACQUITY UPLC BEH C18 column （2.1mm×50mm,1.7μm） was adopted and eluted with a gra- dient program, with acetonitrile-lO mmol ·L^-1NH4HCO3 （pH 10） as the mobile phases. The flow rate was 0. 45 mL · min^-1. The content was determined with ESI and MRM. The results showed that aconitine, hypaconitine and mesaconitine showed a good linear relationship, with r 〉0. 999, within the range of O. 1-100 ng · L^-1. The recoveries were detected to be 100. 1%, 97.4%, 97.5%, with RSD being 1.2%, 1.1%, 1.5%, respectively. This method was used to prove the safety of Shenfu injection, and provide scientific basis for correct evaluation of curative effect of monkshood, as well as a reliable, simple and practical means for quality control of monkshood-containing Chinese materia medica preparations.

关 键 词：乌头碱 次乌头碱 新乌头碱 参附注射液 中空纤维液相微萃取 超高效液相色谱质谱 

分 类 号：R286.0[医药卫生—中药学]