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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 optimize the extraction, purification and determination of bisphenol A in milk by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) with bisphenol A (BPA) Quantitative detection methods. Methods Acetonitrile was used as extractant and protein precipitator. The mixed anion solid phase extraction column was used for purification. The samples were detected by UPLC-MS / MS in negative ion mode and quantified by internal standard method. Results The method showed a good linear relationship in the range of 1 ~ 100 μg / L with a correlation coefficient of r2> 0.990. The average recoveries ranged from 92% to 115% at different loading levels in blank milk matrix with relative standard deviations 3.7% ~ 6.6%; lower limit of determination of 1μg / kg. Conclusion This method is sensitive, accurate and reproducible. It is suitable for the determination of bisphenol A in milk samples.