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

中文关键词:  双酚A  超高效液相色谱-串联质谱法  固相萃取  牛奶

英文关键词:bisphenol A  ultra performance liquid chromatography-tandem mass spectrometry  solid phase extraction  milk

中文摘要:

      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1~100 μg/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1 μg/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。

英文摘要:

      Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry 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 with　mixed anion exchange solid-phase extraction column, the residues were detected by ultra performance liquid chromatography-tandem mass spectrometry under multiple reactions monitoring (MRM) mode via negative-ion mode and quantified by an internal standard method. Results The method showed a good linearity over the range of 1~100 μg/L for bisphenol A with r2>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 1 μg/kg. Conclusion This method is highly sensitive, accurate and reproducible, and it can be suitable for the detection of bisphenol A in milk.