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目的应用顶空气相色谱法测定甲型肝炎灭活疫苗中三氯甲烷残留量。方法采用毛细管色谱柱DB-WAX(30m×0.53mm×0.50μm),ECD检测器,以氮气为载气,顶空进样。以不同基质稀释的三氯甲烷工作液绘制标准曲线,并对方法进行适用性及专属性、线性关系、精密度、定量限、检出限和准确性验证。结果通过绘制的2条标准曲线可见,存在基质效应的影响。甲肝疫苗中三氯甲烷与其他杂质峰的分离度为2.58;三氯甲烷在20～100ng/ml的浓度范围内线性关系良好(R2=0.9993);精密性良好,检测结果的RSD均小于5%;最低检出限为1.2ng/ml,最低定量限为4.8ng/ml;检测高、中、低3种浓度样品的加标回收率分别为(95.6±1.8)%、(95.5±3.1)%和(101.9±2.1)%。结论顶空气相色谱法简便灵敏,结果准确可靠,适用于甲型肝炎灭活疫苗中三氯甲烷残留量的测定。
Objective To determine the residual amount of trichloromethane in hepatitis A inactivated vaccine by headspace gas chromatography. Methods capillary column DB-WAX (30m × 0.53mm × 0.50μm), ECD detector with nitrogen as the carrier gas, headspace injection. The calibration curve was drawn from chloroform working fluid diluted with different matrix. The method was applied to verify the applicability and specificity, linearity, precision, limit of quantification, detection limit and accuracy. Results drawn by the two standard curve shows that there is a matrix effect. The separation of chloroform and other impurity peaks in Hepatitis A vaccine was 2.58. The linearity of chloroform in the concentration range of 20-100 ng / ml was good (R2 = 0.9993). The precision was good. The RSD of the results was less than 5% ; The lowest detection limit was 1.2ng / ml, the lowest limit of quantification was 4.8ng / ml; the recoveries of the spiked samples were (95.6 ± 1.8)%, (95.5 ± 3.1)% And (101.9 ± 2.1)%. Conclusion Headspace gas chromatography is simple and sensitive, the results are accurate and reliable, suitable for determination of trichloromethane residues in hepatitis A inactivated vaccine.