LC/MS法测定氯硝西泮的有关物质  

Determination of clonazepam′s related substances by LC-MS

作　　者：杜宁[1,2] 李忠红[1] 蔡美明[1] 王玉[1,2] 狄斌[2] 

机构地区：[1]江苏省食品药品检验所,南京210008 [2]中国药科大学药物分析教研室,南京210009

出　　处：《药学与临床研究》2009年第5期357-360,共4页Pharmaceutical and Clinical Research

基　　金：国家科技支撑计划子课题(2008BAI55B05-001)

摘　　要：目的：建立氯硝西泮有关物质的LC—UV和LC—MS测定法。方法：液相色谱以C8柱为固定相；以水-甲醇（37：63）为流动相；检测波长为254nm。质谱离子源为ESI，样品采用MS和MS／MS全扫描两种模式进行分析。结果：杂质A和B分别在0．366mg·L^-1～5．860mg·L^-1，0．301mg·L^-1～4．820mg·L^-1范围内线性关系良好，相关系数分别为0．9999、0．9999，最低检测限为1．099ng、0．904ng，杂质A和B的低、中、高3种浓度的平均回收率分别为99．2％、100．2％、100．5％和100．1％、99．7％、99．6％。结论：HPLC法准确、简便，专属性强，可用于氯硝西泮有关物质的考察.Objective： To establish a high performance liquid chromatography-UV and liquid chromatography-mass spectrometry method for the determination of clonazepam＇s related substances. Methods： The chromatography was accomplished on a Cs column, with the mobile phase contain watermethanol （37： 63）, and the detection wavelength was set at 254 nm. The ionic source was ESI. Samples were analyzed in two modes： MS and MS/MS full scan modes. Results： A good relationship was observed in the concentration range of 0. 366 mg·L^-1 -5. 860 mg·L^-1（ impurity A） ,0. 301 mg·L^-1 4. 820 mg·L^-1 （ impurity B）, with the coefficient of 0. 999 （ impurity A） and 0. 999 （ impurity B）. The limit of detection （LOD） was 1. 099 ng （impurity A） and 0. 904 ng （impurity B）. The average recovery of three concentrations were 99.2% , 100.2% , 100.5% （ impurity A） and 100.1% ,99.7% , 99.6% （impurity B）, respectively. Conclusions： The method was proved to be aeeurate, sensitive and showed highly specific. It can be applied for related substances of ctonazepam.

关 键 词：高效液相色谱法 串联质谱 氯硝西泮 有关物质 

分 类 号：R927.1[医药卫生—药学]