顶空气相色谱法测定美伐他汀中有机溶剂残留量

目的 建立美伐他汀中有机残留溶剂的测定方法.方法 顶空气相色谱法.色谱条件:采用HB-5(30.0 m×0.32 mm×0.25 μm)硅胶键合毛细管柱;柱温:初始温度为40℃,保持5 min后,升至90℃,升温速率为2℃/min,保持0 min,升至160℃,升温速率为30℃/min,保持2 min;检测器:火焰离子化检测器;进样器温度:220℃;检测器温度:260℃;载气:氮气;流速:4 ml/min;分流比:1:10.结果 丙酮在15.8～79.0μg/ml、乙酸乙酯在18.0～90 μg/ml、甲苯在8.7～43.3 μg/ml范围内峰面积与浓度呈较好线性关系.平均回收率(n=9)分别为丙酮101.0%,相对标准偏差值(RSD)=1.6%;乙酸乙酯99.8%,RSD=1.0%.结论 本方法操作简便、结果准确,是控制美伐他汀中残留溶剂的可靠方法.

Determination of Residual Solvents in Mevastatin by Headspace Gas Chromatography

Objective To establish a method for determination of residue solvent in Mevastatin. Methods Headspace gas chromatography was used. The HB-5 capillary colunm (30.0 m×0.32 mm×0.25 μm) were used; nitrogen was used as the carry gas; the initial temperature of column was 40℃, and kept for 5 min, than turn to 90℃ by the rate of 2℃/min, and after that turn to 160℃ by the rate of 30℃/min and kept for 2 min; the injector was set at 220℃ and FID detector at 260℃; the flow rate was 4 mL/min; the distributary rate was 1: 10. Results The calibration curves for acetone, ethyl-acetate, and toluene were linear in the rang of 15. 8～79. 0 μg/ml, 18. 0～90μg/ml, and 8. 7～43.3μg/ml,respectively. The average recoveries of acetone and ethyl-acetate were 101.0% (RSD=1.6%, n=9) and 99.8% (RSD=1.0%, n=9), respectively. Conclusion This method is easy to operate with precise result, and is a reliable method for the control of residue solvent of Mevastatin.