气相色谱-质谱法测定维拉唑酮原料药中异亚丙基丙酮  

Determination of mesityl oxide in vilazodone bulk drug by gas chromatography-mass spectrometry

作　　者：史迎杰 魏晓晓[1] 张梅[1] 叶能胜[2] Shi Yingjie;Wei Xiaoxiao;Zhang Mei;Ye Nengsheng(Institute of Analysis and Testing,BeiJing Academy of Science and Technology(BeiJing Center for Physical&Chemical Analysis),Beijing 100089,China;Capital Normal University,Beijing 100048,China)

机构地区：[1]北京市科学技术研究院分析测试研究所(北京市理化分析测试中心),北京100089 [2]首都师范大学,北京100048

出　　处：《分析仪器》2024年第4期45-49,共5页Analytical Instrumentation

基　　金：北京市科学技术研究院创新工程项目(24CA001-03)。

摘　　要：使用气相色谱-质谱联用仪(GC-MS),液体进样方式,测定维拉唑酮原料药中异亚丙基丙酮的分析方法。样品经过溶液提取,选用DB-624毛细管色谱柱(30m×0.32mm,1.8μm),采用全扫描模式(SCAN)和选择离子监测模式(SIM)对异亚丙基丙酮进行定性定量分析。结果显示异亚丙基丙酮浓度在0.01mg·L^(-1)~6.00mg·L^(-1)范围内与峰面积呈良好的线性关系(r>0.9999);加标回收率达到90%以上,相对标准偏差小于3%。该方法具有检测灵敏度高、方法普遍性强,标准配置仪器便可实现检测、专属性好、定量结果快速、准确等优点,适合于维拉唑酮原料药中异亚丙基丙酮的测定。To establish a gas chromatography-mass spectrometry(GC-MS)method for the determination of mesityl oxide in vilazodone crude drug by liquid injection.The samples were extracted by solution,and the DB-624 capillary column(30m×0.32mm,1.8μm)was used for qualitative and quantitative analysis of mesityl oxide by full scan mode(SCAN)and selected ion monitoring mode(SIM).There was a good linear relationship between the concentration of mesityl oxide and the peak area in the range of 0.01mg·L^(-1)-6.00mg·L^(-1)(r>0.9999).The recovery rate of standard addition was over 90%,and the relative standard deviation was less than 3%.The method has the advantages of high detection sensitivity,strong method universality,good specificity,rapid and accurate quantification,etc.

关 键 词：气相色谱-质谱(GC-MS) 异亚丙基丙酮 维拉唑酮 原料药 基因毒性杂质 

分 类 号：TQ460.72[医药卫生—药物分析学] O657.63[化学工程—制药化工]