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  

Determination of four kinds of environment estrogen in drinks by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：林胜军[1] 周日东[1] 黄诚[1] 卢丽明[1] 刘国平[1] 丘福保[1] 黄莉莉[1] 陈夏威[1] 

机构地区：[1]中山市疾病预防控制中心,中山528403

出　　处：《食品安全质量检测学报》2018年第3期614-620,共7页Journal of Food Safety and Quality

基　　金：中山市科技计划项目(2015SYF0104)~~

摘　　要：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,1.8μm)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2~100μg/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、0.01μg/L,在0.25、2、8μg/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10~500μg/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、0.9μg/L,在1.25、10、40μg/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（r0.999）, 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（r0.999）, 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.

关 键 词：超高效液相色谱-串联质谱 饮料 环境类雌激素 

分 类 号：O657.63[理学—分析化学] TS27[理学—化学]