同位素内标-气相色谱-质谱法同时测定婴幼儿配方粉中3-氯丙醇酯和缩水甘油酯的含量

Simultaneous Determination of 3-Monochloropropane-1,2-Diol Esters and Glycidyl Esters in Infant Formula Powder by Isotope Internal Standard-Gas Chromatography-Mass Spectrometry

建立同时测定婴幼儿配方粉中3-氯丙醇酯和缩水甘油酯含量的方法,并检测我国市售部分婴幼儿配方粉中3-氯丙醇酯和缩水甘油酯的含量。结果表明,在最优条件下,3-氯丙醇酯和缩水甘油酯在0.050~0.80 mg/L范围内呈现良好的线性关系,R2均大于0.998,3-氯丙醇酯的加标回收率在81.4%~86.2%,相对标准偏差为4.42%~4.84%,缩水甘油酯的加标回收率为94.5%~101.1%,相对标准偏差为4.46%~6.12%,方法的检出限均为30μg/kg。方法灵敏度高,精密度良好,适用于婴幼儿配方粉中3-氯丙醇酯和缩水甘油酯的定量检测。30份市售婴幼儿配方粉样品中3-氯丙醇酯的含量为50.0~207.8μg/kg,平均值为98.0μg/kg,缩水甘油酯的含量为50.0~480.0μg/kg,平均值为208.1μg/kg。

The aim of this study was the development of a method for the simultaneous determination of 3-monochloropropane-1,2-diol esters(3-MCPDEs)and glycidyl esters(GEs)in infant formula milk powder.Commercial infant formulas available on the Chinese market(n=30)were analyzed for 3-MCPDEs and GEs by gas chromatographymass spectrometry(GC-MS).Under the optimized conditions,3-MCPDEs and GEs showed good linearity in the concentration range of 0.050−0.80 mg/L with correlation coefficient(R2)larger than 0.998.The mean recoveries from spiked samples were in the range of 81.4%−86.2%and 94.5%−101.1%with relative standard deviations(RSDs)ranging from 4.42%to 4.84%and from 4.46%to 6.12%for 3-MCPDEs and GEs,respectively.The limit of detection(LOD)of the proposed method was 30μg/kg for both 3-MCPDEs and GEs.This method showed the advantages of high sensitivity,and accuracy,and could be suitable for the simultaneous detection of 3-MCPDEs and GEs in infant formula milk powder.In the 30 infant formula samples,levels of 3-MCPDEs and GEs ranged from 50.0 to 207.8μg/kg and from 50.0 to 480.0μg/kg with an average of 98.0 and 208.1μg/kg,respectively.