毛细管气相色谱法测定瑞舒伐他汀钙中有机溶剂残留量

目的:建立毛细管气相色谱法测定瑞舒伐他汀钙中有机溶剂的残留量.方法:采用HP-FFAP毛细管色谱柱,载气为氮气,流速为6 ml·min-1;分流比为5:1;程序升温;氢火焰离子化检测器(FID),检测器温度250℃,进样口温度200℃;按外标法测定溶剂残留量.结果:乙醇、乙酸乙酯、四氢呋喃和甲苯分别在100.58～1 005.80(r=0.999 9)、102.00～1 020.00(r=0.999 9)、14.66～146.60(r=0.999 9)、19.12～191.20 μg·m1-1(r=0.999 9)范围内,线性关系良好;平均回收率分别为99.1%(RSD=2.0%),98.5%(RSD=1.6%),98.9%(RSD=1.8%),99.2%(RSD=2.1%).结论:该方法专属性好、快速、简单、结果准确,可用于瑞舒伐他汀钙中有机溶剂残留量的测定.

Determination of Residual Organic Solvents in Rosuvastatin Calcium by Capillary GC

Objective:To develop a method for the determination of residual organic solvents in rosuvastatin calcium.Method: The capillary gas chromatography with programming temperature was established with FID detector and HP-FFAP capillary column.The temperature of the injector and the detector was 200℃and 250℃,respectively.The carrier gas was nitrogen with a flow of 6.0 ml ? min^-1.The split ratio was 5:1.The residual organic solvents were determined by external standard method.Result:Ethanol,ethyl acetate,tetrahydrofuran and toluene showed good linearity within the range of 100.58 1 005.80（r =0.999 9）,102.00～1 020.00（r = 0.999 9）,14.66¹46.60（r=0.999 9） and 19.12～191.2μg ? ml^-1（r = 0.999 9） with the average recovery of 99.1%{RSD = 2.0%),98.5%（RSD = 1.6%）,98.9%（RSD = 1.8%） and 99.2%（RSD =2.1%）,respectively.Conclusion:The method is rapid,simple,accurate and suitable for the analysis of residual organic solvents in rosuvastatin calcium.