超高效液相色谱-串联质谱法测定饮料中的4种环境类雌激素
目的 建立超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定饮料中双酚A(bisphenol A, BPA)、双酚S(bisphenol S, BPS)、辛基酚(octylphenol, OP)和壬基酚(nonylphenol, NP)残留量的分析方法。方法 样品经过HLB固相萃取柱净化后, 用ZORBAX SB-Aq柱(3.0 mm×100 mm, 1.8 μm)分离, 以甲醇和5 mmol/L乙酸铵溶液作为流动相进行梯度洗脱, 电喷雾负离子模式(ESI-)电离, 多反应监测模式(multiple reaction monitoring, MRM)进行检测。结果 BPA、BPS在2~100 μg/L范围内线性关系良好(r>0.999), 方法的检出限(S/N=3)为0.3、0.01 μg/L, 在0.25、2、8 μg/L添加水平的回收率分别为78.6%~88.0%, 相对标准偏差(n=6)为1.1%~6.0%; OP、NP在10~500 μg/L范围内线性关系良好(r>0.999), 方法的检出限(S/N=3)为0.7、0.9 μg/L, 在1.25、10、40 μg/kg添加水平的回收率分别为85.5%~107%, 相对标准偏差(n=6)为2.1%~6.6%。结论 该方法简单、灵敏、准确可靠, 适用于饮料中BPA、BPS、OP和NP等环境类雌激素的测定。
Objective To establish a method for determination of bisphenol A (BPA), bisphenol S (BPS), octyl phenol (OP) and nonylphenol (NP) in drinks by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The targets in the samples were purified by HLB composite solid phase extraction column, separated by ZORBAX SB-Aq column (3.0 mm×100 mm, 1.8 μm) with methanol and acetate solution (5 mmol/L) as mobile phase for gradient elution, then detected by UPLC-MS/MS under the electrospray ionization (ESI?) anion ion mode with multiple reaction monitoring (MRM). Results BPA and BPS had good linearity in the range of 2 μg/L to 100 μg/L (r>0.999), and the limits of detection (S/N=3) were 0.3 and 0.01 μg/L, respectively. The average recoveries were 78.6~88.0% at the spiked levels of 0.25, 2 and 8 μg/L with the relative standard deviations (n=6) of 1.1%~6.0%. OP and NP had good linearity in the range of 10 μg/L to 500 μg/L (r>0.999), and the limits of detection (S/N=3) were 0.7 μg/L and 0.9 μg/L, respectively. The average recoveries were 85.5%~107% at the spiked levels of 1.25, 10 and 40 μg/L, while the relative standard deviations (n=6) were 2.1%~6.6%. Conclusion The method is simple, sensitive and accurate, which is suitable for determination of environment estrogen such as BPA, BPS, OP and NP in drinks.
标题：超高效液相色谱-串联质谱法测定饮料中的4种环境类雌激素
英文标题：Determination of four kinds of environment estrogen in drinks by ultra performance liquid chromatography-tandem mass spectrometry
作者：
林胜军 中山市疾病预防控制中心
周日东 中山市疾病预防控制中心
黄诚 中山市疾病预防控制中心
卢丽明 中山市疾病预防控制中心
刘国平 中山市疾病预防控制中心
丘福保 中山市疾病预防控制中心
黄莉莉 中山市疾病预防控制中心
陈夏威 中山市疾病预防控制中心
中文关键词:超高效液相色谱-串联质谱,饮料,环境类雌激素,
英文关键词:ultra high performance liquid chromatography-tandem mass spectrometry,drinks,environment estrogen,
发表日期：2017-12-21
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