摘要
目的利用在线捕集消除本底,同位素稀释技术,建立婴儿配方食品、鸡蛋、畜肉、水产品、罐头及植物油等食品中4-壬基酚、4-正壬基酚、4-辛基酚、4-正辛基酚和双酚A的超高效液相色谱-串联质谱(ultra-performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定方法。方法样品经乙腈超声提取,官能化聚苯乙烯/二乙烯苯固相萃取柱(polarenhanced polymer,PEP)净化,超高效液相色谱-串联质谱进行测定,采用电喷雾电离负离子模式(electronicsprayion,ESI-),多反应监测(multiplereaction monitoring,MRM)内标法定量分析。并对5种待测组分测定中存在的本底及消除方法进行了研究。结果 5种环境类雌激素在浓度为0.5～50μg/L范围时线性关系良好,相关系数(r)>0.999,方法的定量限为0.5μg/kg,在3种加标浓度的平均回收率为80.1%～104.8%,相对标准偏差(relativestandarddeviation,RSD)小于20%。结论该方法在样品处理过程中采用高温烘烤过的玻璃器皿,并利用在线捕集技术等降低本底,且灵敏度高、定性定量准确,适用于婴儿配方食品、畜肉、水产品、罐头及植物油等中5种环境类雌激素的检测。
Objective To establish an analytical method for the simultaneous determination of nonylphenol(NP),4-n-nonylphenol(4-n-NP),4-tert-octyl phenol(OP),4-n-octyl phenol(4-n-OP) and bisphenol A(BPA) in infant formula,egg,meat,aquatic products,canned food and oil by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) after elimination of background with online capture and isotopic dilution technology.Methods The homogenized sample was extracted with acetonitrile,then the extract was cleaned-up by polar enhanced polymer(PEP) column.The analytics were determined in the modes of electrospray positive ionization(ESI-) and multiple reaction monitoring(MRM) with UPLC-MS/MS and quantified by internal standard method.Thebackground of 5 compounds and removal methods were investigated.Results The 5 kinds of environmental estrogens had good linear relationships in the range of 0.5-50 μg/L,and the correlation coefficients were larger than 0.999.The limits of quantification(LOQ) were 0.5 μg/kg.The recoveries of 3 different spiked levels were 80.1%-104.8%,with the relative standard deviations less than 20%.Conclusion By using roast glass ware during sample pre-treatment,and with mobile phase online capture technology,the method can effectively reduce blank value.The method is highly sensitive,qualitative,quantitative and accurate,which is suitable for the determination of nonylphenol,4-n-nonylphenol,4-tert-octyl phenol,4-n-octyl phenol and bisphenol A in infant formula,egg,meat,aquatic products,canned food and oil.
作者
宁霄
金绍明
唐亚利
刘彬丽
曹进
丁宏
NING Xiao;JIN Shao-Ming;TANG Ya-Li;LIU Bin-Li;CAO Jin;DING Hong(National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《食品安全质量检测学报》
CAS
2019年第1期40-47,共8页
Journal of Food Safety and Quality
基金
国家食品药品监督管理总局科研项目(1010040402229)~~
