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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)、19.12～191.20μg·ml~(-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。
Objective: To establish a capillary gas chromatographic method for the determination of residues of rosuvastatin calcium in organic solvents. Methods: The HP-FFAP capillary column was used. The carrier gas was nitrogen and the flow rate was 6 ml · min -1. The split ratio was 5: 1. The programmed temperature was raised. The FID and the detector temperature 250 ℃, inlet temperature 200 ℃; Determination of solvent residue by external standard method. Results: The results showed that ethanol, ethyl acetate, tetrahydrofuran and toluene ranged from 100.58 to 1005.80 (r = 0.999 9), 102.00-1 020.00 (r = 0.999 9), 14.66-146.60 (r = 0.999 9) The average recoveries were 99.1% (RSD = 2.0%), 98.5% (RSD = 1.6%) and 98.9% (RSD = 1.8%), respectively. , 99.2% (RSD = 2.1%). Conclusion: The method is specific, rapid, simple and accurate. It can be used for the determination of residual organic solvents in rosuvastatin calcium.