自动顶空-气相色谱法测定胶囊中9种残留溶剂

目的]建立自动顶空-气相色谱法测定胶囊中9种残留溶剂的分析方法。方法]准确称取样品于顶空瓶中，加入N，N二甲基乙酰胺，加盖密封，放入自动顶空进样器，供气相色谱分析，外标法定量。对不同极性色谱柱进行选择性实验，最终采用DB-624毛细管柱和氢火焰离子化检测器测定，同时对平衡温度和平衡时间等顶空条件以及色谱条件进行优化。结果]9种溶剂在各自的浓度范围内呈良好的线性关系，相关系数为0.9847-9986，平均回收率为84%-105%，相对标准偏差为0.29%-1.72%。结论]该方法简便、快速、灵敏、准确，适合胶囊中9种残留溶剂的测定。

Determination of 9 Residuals in Capsules by Capillary Gas Chromatography with Auto Headspace Sampling

An analytical method was established and described for the quantitative determination of benzene, methylbenzene, o-xylene, m-xylene, ethyl acetate, vinyl cyanide, n-pentane, dichloromethane and ethyl benzene in food packaging materials by headspace capillary gas chromatography. Headspace capillary gas chromatography has been developed. The benzene, methylbenzene, o-xylene, m-xylene, ethyl acetate, vinyl cyanide, n-pentane, dichloromethane and ethyl benzene were collected and isolated from a standard solution or samples using a headspace system, then quantified by capillary GC-FID. The experimental conditions of headspace and GC were optimized. External standards methods were used for quantitative determination. DB-624 capillary column and hydrogen flame ionization detector （FID） were employed. Under the optimal condition, the linear correlation efficient response of the methods were obtained for benzene, methylbenzene, o-xylene, m-xylene, ethyl acetate, vinyl cyanide, n-pentane, dichloromethane and ethyl benzene were in their respective concentration ranges （R1=0.9847, R2=0.9933, R3=0.9918, R4=0.9930, R5=0.9931, R6=0.9959, R7=0.9925, R8=0.9959, R9=0.9986）. The average recoveries were in the range of 84%-105% with relative standard deviations of 0.29%-1.72%. The method was simple and rapid. It was suitable for the determination of residual benzene, methylbenzene, o-xylene, m-xylene, ethyl acetate, vinyl cyanide, n-pentane, dichloromethane and ethyl benzene in food packaging materials.