热脱附和气-质联用测定卷烟包装材料中的酞酸酯  

Thermal Desorption and Gas Chromatography-Mass Spectrometry for Measurement of Phthalates in Cigarette Package Material

作　　者：侯英[1,2] 曹秋娥[3] 谢小光[3] 王保兴 杨勇 徐济仓 杨燕 刘静 

机构地区：[1]云南瑞升烟草技术(集团)有限公司 [2]云南大学化学系,昆明市650091 [3]云南大学化学系

出　　处：《光谱实验室》2006年第5期1022-1025,共4页Chinese Journal of Spectroscopy Laboratory

摘　　要：建立热脱附-气相色谱-质谱的方法对卷烟包装材料中的酞酸酯(邻苯二甲酸二乙酯、邻苯二甲酸二异丁酯、邻苯二甲酸二正丁酯和邻苯二甲酸正丁正辛酯)进行测定,采用正交实验优化了热脱附条件,优化条件为卷烟包装材料在100℃的热脱附系统(TDS)中热脱附4min,目标物随流量为50mL/min的载气进入-50℃的冷进样系统(CIS4)中冷却,脱附结束后CIS4升温至200℃将目标物挥发进入GC-MS中进行分离和鉴定。采用外标法进行定量,所得校准曲线的线性关系良好,4种酞酸酯在100℃时脱附2min的加标平均回收率范围为80%—90%,相对标准偏差分别为2.07%、3.57%、2.21%和6.38%。该方法样品用量少,前处理简单,重现性较好,可用于卷烟包装材料中酞酸酯的同时测定。A novel method for the determination of phthalates [diethyl phthalate, bis （2- methylpropyl） phthalate, dibutyl phthalate and butyl octyl phthalate] in cigarette package material were estabilished by using thermal desorption coupled to gas chromatography-mass spectrometry （GCMS）. The different parameters affecting thermal desorption were investigated using orthogonal design. The optimized conditions consist of a thermal desorption carried out at 100℃ for 4 min under a helium flow of 50mL/min while maintaining a cryofocusing temperature of -50℃ in the programmed temperature, vaporisation injector （CIS-4）of the GC-MS system. Finally, the PTV injector was ramped to a temperature of 200℃ and the analytes were separated in the GC and detected by MS using full scan mode （m/Z, 35-400）. The quantitative analysis was performed with external standard method. Good linearities were obtained for 4 kinds phthalates. The relative standard deviations（RSDs）of the four phthalates were 2. 07%-6.38% with the recoveries of 80%-90%. The method shows the advantages of small sample size, simple pretreatment, high precision and sensitivity,and can be used as a powerful tool for the analysis of the phthalates in cigarette package material samples.

关 键 词：热脱附 酞酸酯 卷烟包装材料 气-质联用 

分 类 号：O657.63[理学—分析化学]