超高效液相色谱-串联质谱法检测牛奶中双酚A
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。
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.
标题：超高效液相色谱-串联质谱法检测牛奶中双酚A
英文标题：Determination of bisphenol A residues in milk by ultra performance liquid chromatography-tandem mass spectrometry
作者：
张建莹 深圳出入境检验检疫局食品检验检疫技术中心深圳市食品安全检测技术研发重点实验室
杨修斌 深圳出入境检验检疫局食品检验检疫技术中心深圳市食品安全检测技术研发重点实验室
罗耀 深圳出入境检验检疫局食品检验检疫技术中心深圳市食品安全检测技术研发重点实验室
金晓蕾 深圳出入境检验检疫局食品检验检疫技术中心深圳市食品安全检测技术研发重点实验室
岳振峰 深圳出入境检验检疫局食品检验检疫技术中心深圳市食品安全检测技术研发重点实验室
陈波 深圳出入境检验检疫局食品检验检疫技术中心深圳市食品安全检测技术研发重点实验室
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,
发表日期：2014-10-13
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