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

中文关键词:  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

英文关键词:bisphenol-diglycidyl ethers  egg  pork  ultra performance liquid chromatography-tandem mass spectrometry  endocrine disruptors

中文摘要:

      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0.5~100.0 μg/kg浓度范围内线性关系良好, 相关系数(r2)大于0.99。方法的检出限为0.1~0.5 μg/kg, 定量限为0.5~1.0 μg/kg; 在定量限、2.0、 10.0 μg/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0.020~6.450 μg/kg。4批次样品中检出BADGE·H2O·HCl, 检出率为14.29%, 浓度范围为0.26~0.42 μg/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。

英文摘要:

      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?100.0 μg/kg, and the correlation coefficient (r2) was greater than 0.99. The limits of detection were 0.1?0.5 μg/kg, and the limits of quantitation were 0.5?1.0 μg/kg; at the limits of quantitation, 2.0 and 10.0 μg/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?6.450 μg/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?0.42 μg/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.