分析化学2012，Vol.40Issue(2)：304-308,5.DOI:10.3724/SP.J.1096.2012.10582
液相色谱-串联质谱法测定饮料中邻苯二甲酸二(2-乙基)己酯和邻苯二甲酸二异壬酯
Determination of Di (2-ethylhexyl) phthalate and Diisononyl Phthalate Residues in Drinks by High Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A high performance liquid chromatography-tandem mass spectrometric ( HPLC-MS/MS) method was established for the determination of residues of phthatate esters(PAEs), including di(2-ethylhexy1)phthalate (DEHP) and diisononyl phthalate (DINP) in drinks. 2. 0 g drink was shaken and extracted with 8 mL methanol. The extract was added to l0mL methanol and centrifuged . The supermatant was filtered by filter membrane. Then the DEHP and DINP were identified in multiple reactions monitoring (MRM) mode by the mass spectrometry with electrospray in positive ionization mode. The linear range for DEHP was 2 - 200 μg/L and DINP was 10 - 1000 μg/L, with the correlation coefficients (r2) more than 0. 998. No significant matrix effect was found for spiked samples. The recoveries of DEHP and DINP spiked in drinks were 86. 2% - 111. 6% at spiked levels of 0. 01 - 5 mg/kg. The relative standard deviations (RSDs) were less than 11. 0%. The limits of quantization (LOQs) were 0. 01 mg/kg for DEHP, 0. 05 mg/kg for DINP. The proposed procedure was applied to the analysis of 63 real samples from Xiamen, Fujian province (China), of which 34 positive samples were found. This method was sensitive and accurate for the determination of DEHP and DINP in drinks.关键词
液相串联质谱法/邻苯二甲酸酯/基体效应/残留/饮料Key words
High performance liquid chromatography-tandem mass spectrometry/ Diisononyl phthalate/ Di(2-ethylhexyl)phthalate/ Matrix effect/ Residue/ Drink引用本文复制引用
徐敦明,郑向华,杨黎忠,方恩华,陈鹭平,林立毅,周昱..液相色谱-串联质谱法测定饮料中邻苯二甲酸二(2-乙基)己酯和邻苯二甲酸二异壬酯[J].分析化学,2012,40(2):304-308,5.基金项目
本文系国家质检总局行业标准制修订计划项目(2011B341J)和厦门出入境检验检疫局科技项目(No.2011xk005)资助 （2011B341J）
