多种色谱联用技术分析替曲朵辛  

Analysis of tetrodotoxin by hyphenated chromatographic techniques

作　　者：代秀梅[1,2] 于风平 张启明[2] 

机构地区：[1]山东省淄博市食品药品检验所,淄博255086 [2]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2013年第6期983-988,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立替曲朵辛原料药含量及有关物质的测定方法,并对有关物质的结构进行分析。方法:采用HPLC法测定替曲朵辛原料药含量及有关物质,采用UPLC-UV-MS/MS和LC-NMR联用技术对含量最高的杂质9的结构进行分析。结果:重复性好,替曲朵辛浓度在0.294～44.16μg.mL-1范围内线性关系良好(r=0.9999),有关物质中最大杂质为4,9,10,11二脱水河豚毒素。结论:本方法操作简便,结果准确,可作为替曲朵辛原料药含量测定和有关物质检查的方法。Objective：To establish a hyphenated chromatographic method for content determination of tetrodotoxin （TTX） raw medicine and related substances and to analyze the structure of related substances. Methods：HPLC was used to determin the content of tetrodotoxin raw medicine and related substances, and UPLC-UV-MS/MS and LC-NMR were used to study the structure of related substances. Results ：There was a good linear relationship for tetrodotoxin in the range of 0. 294 -44. 16 μg.mL^-1 （r =0. 9999）. The impurity of the highest content was 4,9,10,11 -dianhydro-TTX. Conclusion ：The method is simple, accurate, and well reproducible which can be applied to content determination of Tet-rodotoxin raw medicine and related substances.

关 键 词：替曲朵辛 原料含量测定 有关物质 杂质分析 二脱水河豚毒素 高效液相色谱 液相色谱-串联质谱 液相色谱-核磁联用 

分 类 号：R917[医药卫生—药物分析学]