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

Simultaneous Determination of Residual Trichloromethane and Toluene Contents in Adsorbed DTP Vaccine and The Relevant Biologics by Gas Chromatography

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 determine the residual trichloromethane and toluene contents in adsorbed DTP vaccine and the relevant biologics simultaneously by capillary gas chromatography. Methods HP-5 chromatographic column was used, and the temperatures of injection port, detector and column were set up as 200, 250 and 40℃, while injection volume and split ratio as 1 μl and 10 ∶ 1, respectively. The carrier gas flow rate was optimized, the exclusivity test and locations with trichloromethane and toluene were performed, and the minimum detection limit and quantitative limit were determined. The method was tested for linearity, reproducibility and accuracy, and used for determination of test samples. Results The optimal carrier gas flow rate for chromatography was 1 ml / min. Under the optimal condition for chromatography, good separation effects of trichloromethane and methyl benzene were observed. The minimum detection limits of trichloromethane and toluene were 0. 50 and 0. 38 μg / ml, while the minimum quantitative limits were 2. 10 and 1. 12 μg / ml, respectively. The method showed good reproducibility and linearity. The correlation coefficient was not less than 0. 999 5. The mean recovery rates of trichloromethane and toluene were 102. 9% and 100. 8% respectively. The residual contents of trichloromethane and toluene in 6 batches of products met the relevant requirements. Conclusion Gas chromatography may be used for simultaneous determination of residual trichloromethane and toluene contents in biologics such as adsorbed DTP vaccine.