固相萃取-超高效液相色谱串联三重四级杆质谱法同时测定禽蛋中双酚A、双酚F和双酚S

Determination of Bisphenol A,Bisphenol F,and Bisphenol S in Egg by Solid Phase Extraction-Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

目的建立液相色谱串联三重四级杆质谱法检测禽蛋中双酚A、双酚F和双酚S方法。方法样品采用乙腈提取,使用Oasis HLB固相萃取小柱净化,通过C18色谱柱分离,甲醇-水为流动相,采用电喷雾负离子模式和多反应监测模式检测,内标法定量。结果双酚A和双酚F在1.0~50μg/kg浓度范围呈线性关系(r≥0.999),检出限为0.3μg/kg,定量限为1.0μg/kg;双酚S在0.1~20μg/kg浓度范围呈线性关系(r≥0.999),检出限为0.05μg/kg,定量限为0.15μg/kg。利用该方法测定禽蛋中双酚A、双酚F和双酚S,加标回收率为86.7%~106.3%,相对标准偏差(RSD)为3.1%~7.2%。结论该方法快速便捷、准确稳定,可以满足禽蛋中双酚A、双酚S和双酚F的检测需求。

Objective A method for the determination of bisphenol A,bisphenol F and bisphenol S in egg by liquid chromatography tandem mass spectrometry.Methods The sample was extracted with acetonitrile,purified by Oasis HLB solid phase extraction column.The separation was performed using a C18 column with methanol-water as mobile phase.Detected was operated by electrospray ionization mass spectrometry in negative mode and multi-reaction monitoring mode,and quantified by internal standard method.Results Good linearity was obtained in a range of 1.0~50μg/kg for bisphenol A and bisphenol F(r≥0.999).The detection limit was 0.3μg/kg and the quantitative limit was 1.0μg/kg.Good linearity was obtained in a range of 0.1~20μg/kg for bisphenol S(r≥0.999).The detection limit was 0.05μg/kg and the quantitative limit was 0.15μg/kg.The method was used to determine bisphenol A,bisphenol F and bisphenol S in egg.The recovery was 86.7%~106.3%,and the relative standard deviation(RSD)was 3.1%~7.2%.Conclusion The method is rapid,convenient,accurate and stable,and it is suitable for the determination of bisphenol A,bisphenol F and bisphenol S in egg.