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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 for the simultaneous determination of 17 phthalates (PAEs) in plastics by gas chromatography-negative chemical ionization mass spectrometry (GC-NCI / MS) was established. Plastic samples were extracted with methylene chloride and filtered for detection. The filtrate was chromatographed on a HP-5 MS capillary column at programmed temperature with negative chemical ionization (NCI) mode for mass spectrometry and ammonia gas for the reaction gas. The correlation coefficients (r) of 17 PAEs in the range of 0.05-3.5 mg / L were all above 0.995 with the detection limits of 0.018-2.162 mg / kg. Under the four addition levels of 100, 500, 1000 and 5000 mg / kg, The average recoveries of 17 PAEs ranged from 95.8% to 106.5% with RSD (n = 6) from 2.6% to 7.9%. The method can be used for the detection of 17 kinds of phthalates in plastic products.