分析化学Issue(12)：1811-1817,7.DOI:10.11895/j.issn.0253-3820.140892
在线固相萃取-超高效液相色谱-串联质谱法测定乳制品中双酚A等4种内分泌干扰物
Determination of 4 Environmental Endocrine Disruptors Involving Bisphenol A in Dairy Products by On-line Solid Phase Extraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A simple analytical method by means of on-line solid phase extraction followed liquid chromatography-tandem mass spectrometry ( SPE-LC-MS/MS) was developed for the simultaneous quantitation of 4 endocrine disruptors ( triclosan, triclocarban, bisphenol A and nonylphenol) in dairy products. Infant formula and milk samples were dissolved in acetic acid buffer and hydrolyzed by β-glucuronidase/arylsulfatase. Acetonitrile was used as the extract. Then, the mixture was freeze-centrifuged for 10 min and the supernatant was diluted with water, and analyzed via on-line SPE-LC-MS/MS. The sample extracts were concentrated by an Xbridge C8 cartridge and separated on a BEH C18 column with a gradient mobile phase of methanol and water; then analyzed by triple quadrupole mass spectrometry. Mass acquisition was conducted under negative electrospray ionization mode. Quantification was performed by isotopic internal standard calibration. Acceptable linearity (R2>0. 99) was achieved over the range of 0. 005-5. 0 μg/L, with limits of quantification of 0. 03-1. 0μg/kg. Average recoveries of four target compounds (spiked at three concentration levels) ranged from 80. 2%-106. 7%,with relative standard deviation less than 15%. Due to its rapidity, simplicity, and high sensitivity, the method is suitable for the analysis of endocrine disruptors in dairy products. It has been applied in the analysis of raw milk and milk products collected in Beijing. As a result, nonylphenol was found with a high detectable frequency.关键词
乳制品/三氯生/双酚A/壬基酚/在线固相萃取/液相色谱-串联质谱Key words
Dairy products/Triclosan/Bisphenol A/Nonylphenol/On-line solid phase extraction/liquid chromatography-tandem mass spectrometry引用本文复制引用
张品,张晶,陈洁君,段鹤君,邵兵..在线固相萃取-超高效液相色谱-串联质谱法测定乳制品中双酚A等4种内分泌干扰物[J].分析化学,2014,(12):1811-1817,7.基金项目
本文系质检总局公益性行业科研专项(No.2012104003-03)和国家自然科学基金(No.21177014)资助项目@@@@This work was supported by the National Natural Science Foundation of China (No.21177014) （No.2012104003-03）
