超高效液相色谱-串联质谱法检测牛奶中双酚A

Determination of bisphenol A residues in milk by ultra performance liquid chromatography-tandem mass spectrometry

目的通过优化牛奶中双酚A提取纯化和测定条件,建立牛奶中双酚A(bisphenol A,BPA)的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)定量检测方法。方法 采用乙腈作为提取剂和蛋白质沉淀剂,混合型阴离子固相萃取柱净化,采用UPLC-MS/MS在负离子模式下检测,内标法定量。结果该方法在1~100μg/L范围内有良好的线性关系,相关系数r2】0.990,在空白牛奶基质中,不同添加水平下方法的平均回收率范围为92%~115%,相对标准偏差为3.7%~6.6%;测定低限为1μg/kg。结论 此方法灵敏度高、准确、重现性好,适用于牛奶样品中双酚A的检测。

Objective To establish an ultra performance liquid chromatography-tandem mass spectrome-try method for the determination of bisphenol A (BPA) in milk.Methods The residues of bisphenol in the test samples were extracted with acetonitrile. After being cleaned up withmixed anion exchange solid-phase ex-traction column, the residues were detected by ultra performance liquid chromatography-tandem mass spec-trometry under multiple reactions monitoring (MRM) mode via negative-ion mode and quantified by an internal standard method.ResultsThe method showed a good linearity over the range of 1~100μg/L for bisphenol A withr2>0.990. The average recoveries were 92%~115% at three spiked levels in milk and the relative standard deviations were 3.7%~6.6%. The limit of quantitation was 1μg/kg.ConclusionThis method is highly sensi-tive, accurate and reproducible, and it can be suitable for the detection of bisphenol A in milk.