食品科学 ›› 2023, Vol. 44 ›› Issue (8): 337-344.doi: 10.7506/spkx1002-6630-20220419-240

• 安全检测 • 上一篇    下一篇

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

郝宇, 马艺荧, 于力涛, 李广志, 魏志春, 刘树萍, 石长波   

  1. (1.哈尔滨商业大学旅游烹饪学院,黑龙江 哈尔滨 150028;2.黑龙江省绿色食品科学研究院,黑龙江 哈尔滨 150000)
  • 出版日期:2023-04-25 发布日期:2023-05-06
  • 基金资助:
    黑龙江省科学基金项目(LH2021B015);烹饪科学四川省高等学校重点实验室资助项目(PRKX201906); 2019年度哈尔滨商业大学“青年创新人才”支持计划学术骨干项目(2019CX18); 第二批国家级职业教育教师教学创新团队课题研究项目(ZH2021080101)

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

HAO Yu, MA Yiying, YU Litao, LI Guangzhi, WEI Zhichun, LIU Shuping, SHI Changbo   

  1. (1. College of Toursim and Cuisine, Harbin University of Commerce, Harbin 150028, China; 2. Heilongjiang Academy of Green Food Science, Harbin 150000, China)
  • Online:2023-04-25 Published:2023-05-06

摘要: 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 0~4.00 μg/mL、3-氯丙醇酯含量在0.020 0~2.00 μg/mL的范围内线性良好,相关系数R2>0.999,检出限均为10.0 μg/kg,定量限均为25.0 μg/kg。在25.0、100、300 μg/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~52.4 μg/kg,平均检出值为29.8 μg/kg。缩水甘油酯检出率为6.67%,含量为ND~40.1 μg/kg,平均检出值为31.9 μg/kg。3-氯丙醇酯的平均暴露水平为0.33~0.66 μg/(kg·d),婴幼儿配方乳粉中3-氯丙醇酯和缩水甘油酯污染问题值得重视。

关键词: 3-氯丙醇酯;缩水甘油酯;气相色谱-串联质谱法;婴幼儿配方乳粉

Abstract: 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.

Key words: 3-chloropropanol esters; glycidyl esters; gas chromatography-tandem mass spectrometry; infant formula milk powder

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