超高效液相色谱-串联质谱法同时检测鸡蛋和猪肉中9种双酚-二缩水甘油醚类内分泌干扰物  

Simultaneous determination of 9 kinds of bisphenol-diglycidyl ethers endocrine disruptors in egg and pork by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：古丽努尔·木哈依 危玲[3] 张晶[2] 李会 GULINUER Mu-Ha-Yi;WEI Ling;ZHANG Jing;LI Hui(Microbiological Laboratory,Urumqi Municipal Center for Disease Control and Prevention,Urumqi 830000,China;Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning,Beijing Center for Disease Prevention and Control,Beijing 100013,China;Department of Obstetrics,Beijing Obstetrics and Gynecology Hospital,Capital Medical University,Beijing 100020,China)

机构地区：[1]乌鲁木齐市疾病预防控制中心微生物检验科,乌鲁木齐830000 [2]北京市疾病预防控制中心食物中毒诊断溯源技术北京市重点实验室,北京100013 [3]首都医科大学附属北京妇产医院,北京100020

出　　处：《食品安全质量检测学报》2021年第21期8420-8426,共7页Journal of Food Safety and Quality

基　　金：国家重点研发计划项目(2017YFC1600501)。

摘　　要：目的建立可同时检测鸡蛋和猪肉中9种双酚-二缩水甘油醚(bisphenol-diglycidyl ethers,BDGEs)类内分泌干扰物的超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)。方法样品经磷酸盐缓冲液稀释后,用0.1%甲酸乙腈溶液进行提取,然后用正己烷除脂,Oasis PRiME HLB固相萃取柱净化,在电喷雾电离正离子模式下使用超高效液相色谱-串联质谱仪进行检测,内标法定量。结果鸡蛋和猪肉样品中9种BDGEs类物质在0.5~100.0μg/kg浓度范围内线性关系良好,相关系数(r^(2))大于0.99。方法的检出限为0.1~0.5μg/kg,定量限为0.5~1.0μg/kg;在定量限、2.0、10.0μg/kg 3个添加水平下,鸡蛋和猪肉样品中9种BDGEs类物质的平均回收率为80.16%~115.27%,日内变异系数为2.13%~11.15%,日间变异系数为7.24%~18.62%。采用该方法对28份市售鸡蛋样品进行分析,10批次样品中检出BADGE·2H2O,检出率为35.71%,浓度范围为0.020~6.450μg/kg。4批次样品中检出BADGE·H2O·HCl,检出率为14.29%,浓度范围为0.26~0.42μg/kg。结论本方法具有较高的灵敏度和准确度,适用于动物性食品中9种BDGEs类内分泌干扰物残留量的同时检测和准确定量。Objective To establish a method for the simultaneous detection of 9 kinds of bisphenol-diglycidyl ethers(BDGEs)endocrine disruptors in egg and pork by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were diluted with phosphate buffer solution and extracted with 0.1%formic acid-acetonitrile solution,and the samples were degreased by n-hexane,purified by Oasis PRiME HLB solid phase extraction column,and detected by ultra performance liquid chromatography-tandem mass spectrometry in positive ion mode of electrospray ionization using internal standard method for quantification.Results The linear relationships of the 9 kinds of BDGEs in egg and pork samples were good within the concentration range of 0.5-100.0μg/kg,and the correlation coefficient(r^(2))was greater than 0.99.The limits of detection were 0.1-0.5μg/kg,and the limits of quantitation were 0.5-1.0μg/kg;at the limits of quantitation,2.0 and 10.0μg/kg levels,the average recoveries of the 9 kinds of BDGEs in egg and pork samples were 80.16%-115.27%,the intra-day coefficient of variation were 2.13%-11.15%,and the intra-day coefficient of variation were 7.24%-18.62%.A total of 28 commercial egg samples were analyzed by this method,BADGE·2H2O was detected in 10 batches of samples,with the detection rate of 35.71%and the concentration ranges were 0.020-6.450μg/kg.BADGE·H2O·HCl was detected in 4 batches of samples,with the detection rate of 14.29%and the concentration ranges were 0.26-0.42μg/kg.Conclusion This method has high sensitivity and accuracy,and is suitable for simultaneous detection and accurate quantification of 9 kinds of BDGEs endocrine disruptors residues in animal food.

关 键 词：双酚-二缩水甘油醚 鸡蛋 猪肉 超高效液相色谱-串联质谱法 内分泌干扰物 

分 类 号：O657.63[理学—分析化学] TS253.7[理学—化学] TS251.7[轻工技术与工程—农产品加工及贮藏工程]