同位素稀释-固相萃取-超高效液相色谱-串联质谱法测定食品中双酚A和双酚S

Determination of bisphenol A and bisphenol S in food by isotope dilution-solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

目的建立食品中双酚A及双酚S残留的同位素稀释-固相萃取-超高效液相色谱-串联质谱测定方法。方法样品加入同位素内标,经乙腈超声提取、ENVI Carb固相萃取柱净化后,以BEH C18(2.1 mm×100 mm,1.7μm)色谱柱分离,甲醇和水为流动相对目标物进行梯度洗脱。在电喷雾负离子多反应监测模式检测,内标法定量。结果双酚A和双酚S分别在0.5μg/L^50.0μg/L和0.1μg/L^10.0μg/L具有良好的线性关系,相关系数均>0.999;双酚A在固态食品和液态食品中的定量限分别为0.6μg/kg和48 ng/L;双酚S在固态食品和液态食品中的定量限分别为0.1μg/kg和7.0 ng/L;低、中、高3个加标水平下,双酚A和双酚S在6类食品基质中的平均回收率为85.0%~108.4%,相对标准偏差(RSD)为0.7%~8.2%。结论该方法重现性好、灵敏度高、定量准确,可满足食品中双酚A和双酚S残留的检测需要。

Objective To develop a method for the determination of bisphenol A and bisphenol S in food by isotope dilution-solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-MS/MS）.Methods The samples were spiked with isotope internal standard,and then extracted with acetonitrile,followed by ENVI Carb column to remove matrix interference. The separation was performed on a BEH C18（ 2. 1 mm × 100 mm,1. 7 μm） column by using methanol and water as mobile phase with gradient elution. Detection was operated by electrospry ionization mass spectrometry in negative mode under multiple reaction monitoring mode,internal standard method was employed for quantitative analysis.Results Good linearity was obtained in a range of 0. 5 μg/L-50. 0 μg/L and 0. 1 μg/L-10. 0 μg/L for BPA and BPS,respectively. The limits of quantitation（ LOQ） for BPA solid foods and liquid foods were 0. 6 μg/kg and 48 ng/L,respectively.The LOQ for BPS in solid foods and liquid foods were 0. 1 μg/kg and 7. 0 ng/L,respectively. The average recoveries of BPA and BPS in six food matrix were within 85. 0%-108. 4%,with relative standard deviations of 0. 7%-8. 2%. Conclusion The developed method is selective,sensitive and accurate,and it is suitable for the determination of trace bisphenol A and bisphenol S in food.