气相色谱-串联质谱法测定婴幼儿配方乳粉中的3-氯丙醇酯和缩水甘油酯及其风险评估

建立检测婴幼儿配方乳粉中3-氯丙醇酯和缩水甘油酯的气相色谱-串联质谱法，测定不同市售婴幼儿配方乳粉中3-氯丙醇酯和缩水甘油酯的含量，掌握婴幼儿配方乳粉中酯类污染情况并进行安全风险评估。采用正己烷提取婴幼儿配方乳粉中的3-氯丙醇酯和缩水甘油酯，经过水解、苯基硼酸衍生、气相色谱-串联质谱法测定，内标法定量。结果表明，3-氯丙醇酯和缩水甘油酯总量在0.040 0～4.00μg/m L、3-氯丙醇酯含量在0.020 0～2.00μg/m L的范围内线性良好，相关系数R²>0.999，检出限均为10.0μg/kg，定量限均为25.0μg/kg。在25.0、100、300μg/kg添加水平下，平均回收率在95.0%～98.1%之间。该方法准确率高、回收率好，可用于婴幼儿配方乳粉中的3-氯丙醇酯和缩水甘油酯的检测。150份市售婴幼儿配方乳粉样品中，3-氯丙醇酯检出率为12.7%，含量为ND～52.4μg/kg，平均检出值为29.8μg/kg。缩水甘油酯检出率为6.67%，含量为ND～40.1μg/kg，平均检出值为31.9μg/kg。3-氯丙醇酯的平均暴露水平为0.33～...

Determination and Health Risk Assessment of 3-Chloropropanol and Glycidyl Esters in Infant Formula Milk Powder by Gas Chromatography-Tandem Mass Spectrometry

A gas chromatography-tandem mass spectrometry (GC-MS/MS) method for the detection of 3-chloropropanol and glycidyl esters in infant formula milk powder was established, and the content of 3-chloropropanol and glycidyl esters in different commercial infant formula milk powders was determined. Ester contamination and health risk assessment in infant formula milk powder was carried out. 3-Chloropropanol and glycidyl esters in samples were extracted with n-hexane, hydrolyzed, derivatized with phenylboronic acid, detected by GC-MS/MS, and quantified by an internal standard method. The results showed that the total amount of 3-chloropropanol and glycidyl esters was in the range of 0.040 0–4.00 μg/mL, and good linearity was observed for 3-chloropropanol esters in the concentration range of 0.020 0–2.00 μg/mL with correlation coefficient (R2) greater than 0.999. The limit of detection (LOD) was 10.0 μg/kg, and the limit of quantification (LOQ) was 25.0 μg/kg for both esters. At spiked levels of 25.0, 100 and 300 μg/kg, the average recoveries ranged from 95.0% to 98.1%. The developed method had high accuracy and recovery, and could be used for the detection of 3-chloropropanol and glycidyl esters in infant formula milk powder. In 150 commercial infant formula milk powder samples, the detection rate of 3-chloropropanol esters was 12.7% at levels of ND–52.4 μg/kg with an average of 29.8 μg/kg. The detection rate of glycidyl esters was 6.67% at levels of ND–40.1 μg/kg with an average of 31.9 μg/kg. The average exposure level to 3-chloropropanol esters was 0.33–0.66 μg/(kg·d). Therefore, attention should be paid to the problem of contamination of 3-chloropropanol and glycidyl esters in infant formula milk powder.