Shao Bing, Han Hao, Tu Xiaoming, Huang Lei
Beijing Center for Disease Control & Prevention, Beijing 100013, China.
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.
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.
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。