摘要
建立生活饮用水中18种邻苯二甲酸酯类化合物(phthalic acid esters,PAEs)残留量的气相色谱-串联质谱(gas chromatography-tandem mass,GC-MS/MS)检测方法。生活饮用水样品经亲水亲酯平衡柱(hydrophilicl pophilibalance,HLB)玻璃小柱富集,二氯甲烷洗脱,采用GC-MS/MS多反应监测模式分析,外标法定量。结果表明,采用优化后条件,18种PAEs在0.02 mg/kg^1.00 mg/kg的定量范围内,线性关系良好,相关系数均在0.998以上。按照建立的方法,分别进行添加浓度为0.02、0.1、0.2 mg/kg的加标回收率试验,18种PAEs的平均回收率范围为71.3%~113%,相对标准偏差小于6.8%。4种色谱纯有机溶剂二氯甲烷、甲醇、正己烷、乙腈浓缩10倍后均检出邻苯二甲酸二异丁酯(diisobutyl phthalate,DIBP)、邻苯二甲酸二丁酯(dibutyl phthalate,DBP)和邻苯二甲酸二(2-乙基己)酯(bis(2-ethylhexyl)phthalate,DEHP)3种PAEs,含量范围为0.006 95 mg/kg^0.323 mg/kg,同时进行多次过程空白试验可排除试剂带入的干扰。本方法富集倍数高、快速、准确,可用于生活饮用水中18种PAEs的实际检测分析。
A gas chromatography-tandem mass spectrometry（GC-MS/MS）was established for the determination of 18 kinds of phthalic acid esters（PAEs）in drinking water. The drinking water was enriched by hydrophilicl pophilibalance（HLB）glass column and eluted with dichloromethane,and then quantified by external standard method in multiple reactions monitoring mode（MRM）. Under the optimized conditions, the target concentrations and peak areas were linearly correlated in the range of 0.02 mg/kg-1.00 mg/kg,and the correlation coefficients were greater than 0.998. Recovery studies were carried out on spiked matrices（the purified water）with 18 PAEs at spiking levels of 0.02,0.1,0.2 mg/kg and the mean recoveries were 71.3 %-113 %,with relative standard deviations less than 6.8 %. Diisobutyl phthalate（DIBP）,dibutyl phthalate（DBP）and bis（2-ethylhexyl）phthalate（DEHP）were detected in four chromatographic pure organic solvents：dichloromethane,methanol,n-hexane and acetonitrile which were concentrated 10 times. The content ranges were 0.006 95 mg/kg-0.323 mg/kg. Multiple process blank tests could eliminate the interference of the reagents.The method has the advantages of high enrichment,fast and accurate,and can be used for the actual detection and analysis of 18 kinds of PAEs in drinking water.
作者
朱萌萌
周敏
陈卢涛
胡松
俞璐萍
黎斌
胡晋峰
王川丕
ZHU Meng-meng;ZHOU Min;CHEN Lu-tao;HU Song;YU Lu-ping;LI Bin;HU Jin-feng;WANG Chuan-pi(Greentown Agricultural Detection Technology Co.,Ltd.,Hangzhou 310000,Zhejiang,China;State Key Laboratory of Tea Plant Biology and Utilization,College of Tea and Food Science ＆ Technology,Anhui Agricultural University,Hefei 230036,Anhui,China)
出处
《食品研究与开发》
CAS
北大核心
2018年第12期130-137,共8页
Food Research and Development
