顶空气相色谱法检测百乐眠胶囊中树脂残留物

Determination of Residual Resin in Bailemin Capsules by Headspace GC Method

建立气相色谱法检测百乐眠胶囊中树脂残留物的方法。采用气相色谱法对百乐眠胶囊中苯、甲苯、二甲苯、正己烷、苯乙烯、 1,4 -二乙苯的残留量进行检测 ,气相色谱条件为 :色谱柱HP - 5 ,载气为高纯氮气 ,柱前压为 10Psi,气化室温度 2 0 0℃ ,柱温 6 0℃ (5min) ,以 30℃·min- 1的速率升至 90℃(3 5min) ,再以 30℃·min- 1的速率升至 14 0℃ (4min) ,最后以 30℃·min- 1的速率升至 190℃ (3min) ,检测器为FID ,温度为 2 2 0℃。正己烷在 1 815～ 2 9 0 6 0 μg·ml- 1,苯在 0 0 12 8～ 0 196 6 μg·ml- 1内 ,甲苯在 0 6 85～ 11 12 5 μg·ml- 1内 ,二甲苯在 1 6 98～ 2 7 170 μg·ml- 1内 ,苯乙烯在 1 6 95～ 2 7 12 5 μg·ml- 1内 ,1,4 -二乙苯在 1 6 99～ 2 7 14 0 μg·ml- 1内均有良好的线性关系 ,相关系数分别为 0 9996、 0 9991、 0 9996、 0 9998、0 996 6、 0 9980。本法简便、快速、准确度高 ,适于测定百乐眠胶囊中树脂残留物 ,可作为百乐眠胶囊的质量监控方法。

A headspace GC method was established for the determination of residual resin including benzene, toluene, xylene, n-hexane, styene and 1,4-diethyl benzene in Bailemin capsules. A HP-5 column was used with high purity nitrogen as carrier gas. Temperature of gasifying compartment was 200℃. Column temperature :60℃, from 60℃ to 90℃ at rising rate of 30℃·min -1 and keeping 3min; then from 90℃ to 140℃ at rising rate of 30℃·min -1 and keeping 3min. FID director and its temperature 220℃. Good linear responses have been obtained in the following range for n-hexane 1.851～29.060μg·ml -1 (r=0.9996), n-hexane 1.851～29.060μg·ml -1 (r=0.9996), benzene 0.0128～0.1966μg·ml -1 (r=0.9991), toluene 0.685～11.125μg·ml -1 (r=0.9996), xylene 1.698～27.170μg·ml -1 (r=0.9998), styrene 1.695～27.125μg·ml -1 (r=0.9966), 1,4-diethyl benzene 1.699～27.140μg·ml -1 (r=0.9980). The method is simple, quick, and accuracy for determination of residual resin in Bailemin capsules and can be used for quality control.