气相色谱法同时测定替格瑞洛片中14种残留溶剂

Determination of 14 residual solvents in the drug of ticagrelor tablets by GC

为建立同时测定替格瑞洛片中14种残留溶剂的方法,采用DB-624(75 m×0.53 mm×3μm)毛细管气相色谱柱,柱流速5.0 mL/min,FID检测器,进样口温度200.0℃,检测器温度250.0℃,分流比为10∶1,正丙醇为内标,内标法定量测定替格瑞洛片中异辛烷、正庚烷、甲苯、N,N-二异丙基乙胺、甲醇、乙醇、乙腈、异丙醇、甲基叔丁基醚、乙酸乙酯、四氢呋喃、二氧六环、乙二醇和二氯甲烷14种溶剂的残留量。结果显示:各成分之间能有效分离,在1.6~124.9μg/mL线性范围内各个化合物线性关系良好(r≥0.9995);回收率为73.6%~122.1%,RSD(n=6)为0.4%~12.2%;定量限为1.0~20.8μg/mL。该方法操作简便、快速、灵敏、高效,可为替格瑞洛片质量标准的提高提供依据。

To establish a GC method for determination of 14 residual organic solvents in Ticagrelor tablets,Isooctane,n-heptane,toluene,N,N-Diisopropylethylamine,methanol,ethanol,acetonitrile,isopropanol,methyl tert-butyl ether,ethyl acetate,tetrahydrofuran,dioxane,ethylene glycol and dichloromethane were determined on DB-624(75 m×0.53 mm×3μm),with the column flow rate of 5 mL/min,FID detector,injection port temperature 200℃,detector temperature 250℃,split ratio 10∶1,n-propanol quantified as internal standard.Results show that the components can be effectively separated,and have a good linear relationship(r≥0.9995)in each linear range(1.6~124.9μg/mL),the average recoveries were 73.6%~122.1%,with RSDs(n=6)of 0.4%~12.2%,The limit of quantification was 1.0~20.8μg/mL.The method is easy,rapid,sensitive,and efficient,and provides a basis for quality standard improvement of ticagrelor tablets.