顶空气相色谱法测定康百汀中有机溶剂残留

Determination of Residual Solvents in Compactin by Headspace Gas Chromatography

目的建立康百汀中残留有机溶剂的测定方法。方法采用顶空气相色谱法。色谱条件:5%苯基-1%乙烯基-94%聚二甲基硅氧烷毛细管柱;内标物:2-己酮;柱温:初始温度为45℃,保持5min后,升至90℃,升温速率为2℃/min,保持0min,升至160℃,升温速率为30℃/min,保持2min;检测器:FID检测器;进样口温度:220℃;检测器温度:260℃;载气:氮气;流速:8ml/min;分流比:10:1。结果 3种残留溶剂在对应于限度的50%～150%浓度范围内,溶剂与内标物质峰面积的比值与浓度呈较好线性关系(r=0.9997～0.9999);平均回收率(n=9)为99.2%～100.2%。结论本方法操作简便、结果准确,可用于康百汀中有机溶剂残留量的测定。

Objective To establish a method for the determination of residual solvents in compactin.Methods Headspace gas chromatography was employed.5% phenyl 1% vinyl 94% dimethyl polysiloxane capillary column was used.2-Hexanone was used as internal standard.The column temperature was 45℃ initially and maintained for 5 min;then,heated up to 90℃ at the rate 2℃/min and maintained for 0 min;afterwards,heated up to 160℃ at the rate of 30℃/min and maintained for 2 min.Detector：flame ionization detector （FID） was used and its temperature was 260℃;temperature of the injector port was 220℃.Nitrogen was used as the carry gas;the flow rate was 8 ml/min;and the distributary rate was 10：1.Results The correlation coefficients of linearity ranged from 0.999 7～0.999 9 for the 3 residual solvents within the concentration of 50%～150% of relative individual limit specified,and the average recovery rates （n=9） were between 99.2%～100.2%.Conclusion This method is easy to operate with precise results,and can be used for determining the residual solvents in compactin.