GC-MS法检测磷酸川芎嗪氯化钠注射液中邻苯二甲酸酯类物质含量

The Research on a GC-MS Method for Simultaneous Determination of Phthalate Plasticizers in Ligustrazine Phosphate and Sodium Chloride Injection

目的:建立气相色谱-质谱联用方法,用于检测磷酸川芎嗪氯化钠注射液中邻苯二甲酸酯类物质含量。方法:色谱柱为DB-5MS,载气为氦气,流速为1.0 m L·min^(-1),进样口温度为260℃,柱温为程序升温。电子轰击电离方式,离子源温度:230℃;定量测定采用MRM模式。以3批磷酸川芎嗪氯化钠注射液为测定对象,测定邻苯二甲酸酯类物质含量。结果:21种邻苯二甲酸酯类分离良好,在80~2000 ng·mL^(-1)浓度范围内呈良好线性关系,检测限>2 ng·mL^(-1),加样回收率为90.7%~97.1%。结论:该法分离效果好、准确性高、灵敏、简便,可用于检测磷酸川芎嗪氯化钠注射液中邻苯二甲酸酯类物质,并能够适应大规模样品的快速分析要求。

Objective:A GC-MS method was established for the determination of 21phthalate plasticizers in Ligustrazine Phosphate and Sodium Chloride Injection.Methods:The determin ation was performed on DB-5MS column at the flow rate of 1.0 mL·min^(-1)using helium as carrier gas,injector temperature was 260℃by temperature programming.Electron impact(EI)ionization mode was used,MRM was used for quantity analysis,the assays of phthalates elasticizers in 3 batches Ligustrazine Phosphate and Sodium Chloride Injection were determined.Results:21 kinds of phthalates could be completely separated under the condition of GC-MS.The linear ranges were 80~2000 ng·mL^(-1).The limit of detection was more than 2 ng·mL^(-1)and average recoveries were 90.7%~97.1%.Conclusion:This work provided an effective,accurate,sensitive and simple method for the rapid detection of huge quantity of samples.