同位素稀释液相色谱－串联质谱法测定食品中的5种环境类雌激素
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(polar enhanced 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(electronic spray ion, ESI-), 多反应监测(multiple reaction 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0.5~50 μg/L范围时线性关系良好, 相关系数(r)＞0.999, 方法的定量限为0.5 μg/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(relative standard deviation, 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. The background 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.
标题：同位素稀释液相色谱－串联质谱法测定食品中的5种环境类雌激素
英文标题：Determination of 5 environmental estrogens in food by isotopic dilution ultra-performance liquid chromatography-tandem mass spectrometry
作者：
宁霄 中国食品药品检定研究院
金绍明 中国食品药品检定研究院
唐亚利 中国食品药品检定研究院
刘彬丽 中国食品药品检定研究院
曹进 中国食品药品检定研究院
丁宏 中国食品药品检定研究院
中文关键词:超高效液相色谱-串联质谱法,4-壬基酚,4-正壬基酚,4-辛基酚,4-正辛基酚,双酚A,
英文关键词:ultra-performance liquid chromatography-tandem mass spectrometry,nonylphenol,4-n-nonylphenol,4-tert-octyl phenol,4-n-octyl phenol,bisphenol A,
发表日期：2018-10-17
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