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目的应用毛细管气相色谱法同时检测吸附百白破疫苗及相关生物制品中三氯甲烷和甲苯的残留量。方法采用HP-5色谱柱,设置进样口温度为200℃,检测器温度为250℃,柱温为40℃,进样体积为1μl,分流比为10∶1。优化色谱载气(氮气)流速进行定位,确定最低检出限和定量限,并进行线性、重复性、准确性(加样回收)试验及样品测定。结果最佳色谱载气(氮气)流速为1ml/min;在确定的色谱条件下,三氯甲烷和甲苯的分离效果良好,最低检出限分别为0.50和0.38μg/ml,最低定量限分别为2.10和1.12μg/ml;重复性好;线性关系良好,相关系数均不低于0.9995;平均回收率分别为102.9%和100.8%。检测的6批制品的三氯甲烷和甲苯的残留量均符合规定。结论气相色谱法可同时检测吸附百白破疫苗等生物制品中三氯甲烷和甲苯的残留量。
Objective To simultaneously detect the residual amount of chloroform and toluene in the adsorption of diphtheria toxoid vaccine and related biological products by capillary gas chromatography. Methods The HP-5 column was used to set the inlet temperature to 200 ℃, the detector temperature to 250 ℃, the column temperature to 40 ℃, the injection volume to 1μl and the split ratio to 10:1. Optimize the chromatographic carrier gas (nitrogen) flow rate to locate, determine the minimum detection limit and limit of quantification, and linearity, repeatability, accuracy (sample recovery) test and sample determination. Results The optimum chromatographic carrier gas (nitrogen) flow rate was 1ml / min. Under the chromatographic conditions, the separation of trichloromethane and toluene was good with the detection limits of 0.50 and 0.38μg / ml, respectively. The minimum limits of quantification were 2.10 and 1.12μg / ml; good reproducibility; good linear relationship, the correlation coefficient of not less than 0.9995; average recovery rates were 102.9% and 100.8%. Tested 6 samples of chloroform and toluene residues are in line with the provisions. Conclusions Gas chromatography can simultaneously detect the residual amount of chloroform and toluene in biological products such as the adsorption baitai broken vaccine.