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0.0400~4.00μg/mL、3-氯丙醇酯含量在0.0200~2.00μg/mL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0.33~0.66μg/(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。
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 0.0400–4.00μg/mL,and good linearity was observed for 3-chloropropanol esters in the concentration range of 0.0200–2.00μg/mL with correlation coefficient(R2)greater than 0.999.The limit of detection(LOD)was 10.0μg/kg,and the limit of quantification(LOQ)was 25.0μg/kg for both esters.At spiked levels of 25.0,100 and 300μg/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–52.4μg/kg with an average of 29.8μg/kg.The detection rate of glycidyl esters was 6.67%at levels of ND–40.1μg/kg with an average of 31.9μg/kg.The average exposure level to 3-chloropropanol esters was 0.33–0.66μg/(kg·d).Therefore,attention should be paid to the problem of contamination of 3-chloropropanol and glycidyl esters in infant formula milk powder.
作者
郝宇
马艺荧
于力涛
李广志
魏志春
刘树萍
石长波
HAO Yu;MA Yiying;YU Litao;LI Guangzhi;WEI Zhichun;LIU Shuping;SHI Changbo(College of Toursim and Cuisine,Harbin University of Commerce,Harbin 150028,China;Heilongjiang Academy of Green Food Science,Harbin 150000,China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2023年第8期337-344,共8页
Food Science
基金
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)。
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
3-chloropropanol esters
glycidyl esters
gas chromatography-tandem mass spectrometry
infant formula milk powder
