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采用基质固相分散萃取和液相色谱-串联质谱法分析鸡蛋和牛奶中的烷基酚和双酚A。

Analysis of alkylphenol and bisphenol A in eggs and milk by matrix solid phase dispersion extraction and liquid chromatography with tandem mass spectrometry.

作者信息

Shao Bing, Han Hao, Tu Xiaoming, Huang Lei

机构信息

Beijing Center for Disease Control & Prevention, Beijing 100013, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2007 May 1;850(1-2):412-6. doi: 10.1016/j.jchromb.2006.12.033. Epub 2007 Jan 12.

Abstract

A method based on matrix solid phase dispersion (MSPD) using C18 as dispersant, and a subsequent cleanup step with amino-propyl solid phase extraction cartridges and liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) has been developed for the simultaneous determination of nonylphenol (NP), octylphenol (OP) and bisphenol A (BPA) in eggs and milk. Recovery studies were performed at different fortification levels. Average recoveries by MSPD varied from 79% of BPA to 98% of NP and relative standard deviations were equal or lower than 15% for egg samples. The average recoveries in milk ranged from 86 to 84% for BPA, 90 to 99% for NP and 82 to 103% for OP and relative standard deviations were equal to or lower than 8%. The limits of detection (LODs) in eggs were 0.10, 0.10 and 0.25 microg/kg for BPA, NP and OP, respectively and LODs for milk were 0.10, 0.05 and 0.10 microg/kg for BPA, NP and OP, respectively. Investigation of the levels in commercial samples indicated that NP was ubiquitous in milk and eggs at levels ranging from 4.24 to 17.60 microg/kg, and the milk samples were more heavily contaminated by NP than were the egg samples.

摘要

已开发出一种基于基质固相分散(MSPD)的方法,该方法使用C18作为分散剂,随后采用氨基丙基固相萃取柱进行净化步骤,并结合液相色谱-电喷雾电离串联质谱(LC-ESI-MS/MS),用于同时测定鸡蛋和牛奶中的壬基酚(NP)、辛基酚(OP)和双酚A(BPA)。在不同加标水平下进行了回收率研究。MSPD法的平均回收率在BPA的79%至NP的98%之间,鸡蛋样品的相对标准偏差等于或低于15%。牛奶中的平均回收率为:BPA为86%至84%,NP为90%至99%,OP为82%至103%,相对标准偏差等于或低于8%。鸡蛋中BPA、NP和OP的检测限(LOD)分别为0.10、0.10和0.25μg/kg,牛奶中BPA、NP和OP的检测限分别为0.10、0.05和0.10μg/kg。对市售样品中含量的调查表明,NP在牛奶和鸡蛋中普遍存在,含量范围为4.24至17.60μg/kg,牛奶样品受NP的污染比鸡蛋样品更严重。

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