气相色谱/质谱联用法测定烟用水基型乳胶中的邻苯二甲酸酯

摘要

为测定烟用水基型乳胶中的邻苯二甲酸酯,用加有内标物质的正己烷溶液对乳胶样品进行了超声萃取,并采用气相色谱/质谱/选择离子监测法(GC/MS/SIM)测定了144个样品中的7种邻苯二甲酸酯:邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基己)酯(DEHP)、邻苯二甲酸二辛酯(DOP)和邻苯二甲酸丁基苄基酯(BBP).结果表明:①样品中加入2 mL水,超声30 min萃取效果较好；②在标准溶液浓度范围内,7种邻苯二甲酸酯的线性均较好,相关系数达到0.996以上；③低、中、高3种浓度的加标回收率在85% ～ 111%之间,相对标准偏差(RSD)均小于5%；④当前国内烟用水基胶中使用的邻苯二甲酸酯类增塑剂主要集中在D1BP,DBP两种.%In order to determine the phthalates in water-based emulsion adhesives for tobacco, the adhesives were extracted with rc-hexane containing internal standard by ultrasonic instruments. Seven phthalates in 144 water-based emulsion adhesive samples, including dimethyl phthalate ( DMP) , diethyl phthalate ( DEP ) , diisobutyl phthalate (DIBP) ,dibutyl phthalate ( DBP) , di-(2-ethylhexyl) phthalate ( DEHP) , dioctyl phthalate (DOP) and benzyl butyl phthalate ( BBP) , were determined by gas chromatography/mass spectrometry. The results showed that;l) 30 minutes were preferable duration for extraction by adding 2 mL water into the sample ;2) the regression coefficients of the 7 phthalates were over 0. 996 within the range of their calibration ;3) the recoveries (the standard spiked at low,middle and high concentration levels) ranged from 85% to 111% ,and the relative standard deviation (USD) of the method was below 5% ;4) DIBP and DBP are the two phthalate plasticizers among the water-based adhesives most commonly used in the cigarette industry.