气相色谱-负化学电离质谱法测定塑料中十七种邻苯二甲酸酯  

Determination of seventeen phthalic acid esters in plastic by gas chromatography-negative chemical ionization mass spectrometry

作　　者：卢瑜[1] 禹伟腾[1] 麦宝华[1] 张斌[1] 梁淑雯[1] 于文杰[1] 

机构地区：[1]深圳出入境检验检疫局,深圳518045

出　　处：《分析试验室》2016年第2期193-196,共4页Chinese Journal of Analysis Laboratory

基　　金：深圳出入境检验检疫局科技项目(SZ2015212)资助

摘　　要：建立了气相色谱-负化学电离质谱法（GC-NCI/MS）同时测定塑料中17种邻苯二甲酸酯（PAEs）的分析方法。塑料样品经二氯甲烷超声提取并过滤后进行检测。采用HP-5 MS毛细管色谱柱在程序升温条件下对滤液进行色谱分离,质谱采用负化学电离（NCI）模式,反应气采用氨气。17种PAEs在0.05-3.5 mg/L范围内线性关系良好,相关系数（r）均大于0.995;检出限为0.018-2.162 mg/kg;在100,500,1000,5000 mg/kg 4个添加水平下,17种PAEs的平均加标回收率为95.8%-106.5%,RSD（n=6）为2.6%-7.9%。方法可用于塑料产品中17种邻苯二甲酸酯的检测。A method was developed for the determination of seventeen phthalic acid esters （PAEs） by gas chromatography-negative chemical ionization mass spectrometry （GC-NCI/MS）. The samples were extracted with dichloromethane by ultrasonic extraction method and filtrated before analysis. The filtrate was separated by HP- 5MS column with temperature programming and the phthalate acid esters were measured by GC-MS in negative chemical ionization （NCI） mode using ammonia as chemical ionization reagent. The seventeen PAEs had a good linear range from 0. 05 mg/L -3.5 mg/L, with the correlation coefficients（r） all above 0. 995. The limits of detection （LOD） of the seventeen PAEs were in the range of 0. 018 - 2. 162 mg/kg. The average recoveries of the seventeen PAEs spiked in plastic at four spiked levels （100,500,1000 and 5000mg/kg） were in the range of 95.8% - 106.5% , and all the relative standard deviations （RSDs） were in the range of 2. 6% - 7.9% （ n = 6）. The developed method is accurate, quick, sensitive and suitable for the determination of the seventeen PAEs in plastic, thus useful for protecting the security of human body and environment.

关 键 词：负化学电离 气相色谱 邻苯二甲酸酯 氨气 塑料 

分 类 号：TQ320.7[化学工程—合成树脂塑料工业]