婴幼儿配方乳粉中氯丙醇酯含量测定方法的研究

Determination method of chloropropanol esters in infant formula

建立气相色谱-质谱法(GC-MS)同时测定婴幼儿配方乳粉中3-氯-1,2-丙二醇酯(3-MCPDE)和2-氯-1,3-丙二醇酯(2-MCPDE)的分析方法。样品中加入氘代同位素内标,经乙酸乙酯提取、甲醇钠-甲醇溶液水解、七氟丁酰基咪唑衍生,气相色谱-质谱法选择离子监测(SIM)模式分析,内标法定量。结果表明,两种化合物在10~400μg/L范围内线性关系良好,相关系数R2>0.999,方法检出限均为0.003 mg/kg,定量限均为0.01 mg/kg;在3个加标浓度水平下的平均回收率为95.8%~115.7%,精密度试验结果的相对标准偏差(RSD)为1.9%~2.2%。该方法简便、快速、准确、灵敏度高,能够满足婴幼儿配方乳粉中氯丙醇酯快速检测的要求。

A method was established for the simultaneous determination of 3-monochloropropane-1,2-diol ester(3-MCPDE)and 2-monochloropropane-1,3-diol ester(2-MCPDE)in infant formula by GC-MS.Infant formula samples were spiked with deuterium-labeled isotope internal standards,extracted with ethyl acetate,and then hydrolyzed by sodium methoxide-methanol solution.After derivatized with N-heptafluorobutyrylimidazole,the samples were analyzed by GC-MS in selected ion monitoring(SIM)mode and quantified by internal standard method.The results showed that the two compounds had a good linear relationship in the range of 10-400μg/L and the correlation coefficients(R2)were more than 0.999.The limit of detection(LDQ)of the method was 0.003 mg/kg,the limit of quantitation(LOQ)of the method was 0.01 mg/kg,the mean standard recovery rate at three spiked samples was in the range of 95.8%-115.7%,and the relative standard deviation(RSD)of precision tests results was 1.9%-2.2%.The method showed the advantages of simpleness,quickness,high accuracy and sensitivity,which could be suitable for the rapid detection of 3-MCPDE and 2-MCPDE in infant formula.