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机构地区:[1]天津市产品质量监督检测技术研究院,天津300384
出 处:《食品安全质量检测学报》2013年第2期444-450,共7页Journal of Food Safety and Quality
摘 要:目的建立婴幼儿配方乳粉中双酚A(BPA)、双酚F(BPF)、己烷雌酚、己烯雌酚、双烯雌酚、辛基酚、壬基酚7种酚类环境激素的液相色谱-串联四极杆质谱检测方法。方法以1%三氯乙酸和乙腈提取,HLB固相萃取净化,由C18液相色谱柱分离,以电喷雾离子源负离子模式,多反应监测(MRM)条件下对7种物质进行检测,基质加标标准曲线法定量。结果 7种化合物检出限在0.5~5μg/kg,定量限从1.5~15μg/kg。7种物质从定量限到50ng/mL范围内线性关系良好。在三水平加标回收试验中,7种化合物的回收率在73.5%~97.9%之间,RSD为5.6%~13.6%。结论本文对7种环境激素同时检测的方法具有准确、高效、灵敏、特异性强等优点,为食品安全风险监控方法提供参考依据。Objective To establish an analytical method for determination of 7 phenolic environmental hormones-Bisphenol A,Bisphenol F,Hexestrol,Diethylstilbestrol,Dienestrol,Octylphenol,and Nonylphenol in infant formulas by liquid chromatography-triple quadrupole mass spectrometry.Methods Samples were extracted with 1% trichloroacetic acid and acetonitrile and purified by HLB solid phase extraction(SPE).The 7 compounds were separated by C18 column and analyzed by LC-MS/MS under multiple reaction monitoring(MRM) mode via negative electrospray ionization,and qualified by curvilinear equations of spiking standard in matrix.Results The limits of determination(LOD) of 7 compounds were 0.5~5 μg/kg,and the limits of quantitation were 1.5~15 μg/kg.The results showed a good linearity over the range of LOQ to 50 ng/mL.The average recoveries of 7 compounds were from 73.5% to 97.9% with the relative standard deviations(RSDs) of 5.6%~13.6% by three-level spiking tests.Conclusion The reported method of analyzing 7 environmental hormones simultaneously has the advantages of accuracy,efficiency,sensitivity and specificity,which will provide references for the risk monitoring of food safety.
分 类 号:TS252.7[轻工技术与工程—农产品加工及贮藏工程]
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