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

建立了饮料中邻苯二甲酸二(2-乙基)己酯(DEHP)和邻苯二甲酸二异壬酯(DINP)残留的液相色谱-串联质谱(LC-MS/MS)检测方法。2.0 g样品经8 mL甲醇振荡提取、定容、离心,取上清液过滤,采用LC-MS/MS电喷雾电离,多反应监测(MRM)模式对样品进行分析。DEHP在浓度范围为2～200μg/L,DINP在10～1000μg/L内线性良好,相关系数均大于0.998。实验表明:样品无明显的基质效应。样品中添加0.01～5 mg/kg的DEHP和DINP,其回收率为86.2%～111.6%;相对标准偏差(n=6)小于11%;DEHP检出限为0.008 mg/kg,定量限为0.01 mg/kg;DINP检出限为0.01 mg/kg,定量限为0.05 mg/kg。本方法提取效果好,具有良好的灵敏度、回收率和重复性,被成功用于实际饮料样品中DEHP和DINP的测定。

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-ethylhexyl）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 10mL 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.