顶空气相色谱法测定美伐他汀中有机溶剂残留量Determination of Residual Solvents in Mevastatin by Headspace Gas Chromatography
杨亚勇,黄炜乾
YANG Ya-yong,HUANG Wei-qian(Livzon New North River pharmaceutical Co.
摘要(Abstract)：
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×0.25μm)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18.0～90μg/ml、甲苯在8.7～43.3μg/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。
Objective To establish a method for determination of residue solvent in Mevastatin.Methods Headspace gas chromatography was used.The HB-5 capillary column(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,18.0～90 μg/ml,and 8.7～43.3 μg/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.
关键词(KeyWords)：
顶空气相色谱法;美伐他汀;残留溶剂
headspace gas chromatography;Mevastatin;residue solvent
基金项目(Foundation):
作者(Author):
杨亚勇,黄炜乾
YANG Ya-yong,HUANG Wei-qian(Livzon New North River pharmaceutical Co.