离子交换固相萃取-气相色谱-质谱联用法测定方便面皮复合包装袋中2,4-二氨基甲苯的迁移量  

Determination of 2,4-diaminotoluene in Mianpi composite packaging film bags by ion-exchange solid-phase extraction-gas chromatography-mass spectrometry

作　　者：芦智远 王冰 田娜 张耀武 张新宇 刘佳 吕岩 LU Zhiyuan;WANG Bing;TIAN Na;ZHANG Yaowu;ZHANG Xinyu;LIU Jia;Lv Yan(Xi’an Supervision & Inspection Institute of Product Quality,Xi’an 710065,China;Xi’an Institute of Measurement and Testing Technology,Xi’an 710086,China)

机构地区：[1]西安市产品质量监督检验院,陕西西安710065 [2]西安计量技术研究院,陕西西安710086

出　　处：《色谱》2019年第10期1053-1058,共6页Chinese Journal of Chromatography

基　　金：国家粮食局行业标准项目(国粮办发[2017]177号)~~

摘　　要：建立了方便面皮复合包装袋中2,4-二氨基甲苯迁移量的离子交换固相萃取-气相色谱-质谱联用检测方法。样品用4%(v/v)乙酸溶液浸泡,然后采用MCX混合型阳离子交换柱富集净化,以5.0mL水淋洗小柱,用3.0mL5%(v/v)氨化甲醇洗脱样品,洗脱液经过溶剂交换,七氟丁酸酐衍生后,用气相色谱-质谱联用仪对目标物进行检测,外标法定量。2,4-二氨基甲苯在1~50μg/L范围内,线性相关系数(r)为0.9991,检出限(S/N=3)为0.2μg/L,定量限(S/N=10)为0.6μg/L,回收率在89.0%~94.2%之间,相对标准偏差为1.9%~3.6%。该方法的前处理过程无需调节提取液的pH值,也不需要液液萃取,大幅简化了前处理过程,降低了有机溶剂的消耗,具有操作便捷、结果准确的优点,适用于方便面皮复合包装袋中2,4-二氨基甲苯迁移量的检测。A method for the determination of 2,4-diaminotoluene in Mianpi composite packaging film bags was established based on ion-exchange solid-phase extraction-gas chromatography-mass spectrometry (GC-MS).The samples were immersed in 4%(v/v) acetic acid solution.2,4-Diaminotoluene was enriched from a 50.0 mL soak solution with an activated and balanced MCX solid-phase extraction column.The MCX column was washed with 5.0 mL water and eluted with 3.0 mL ammoniated methanol.2,4-Diaminotoluene was detected quantitatively by GC-MS after derivatization with heptafluorobutyric acid anhydride.In the mass concentration range of 1-50 μ g/L , the linear correlation coefficient ( r ) was 0.999 1 .The limit of detection (LOD, S/N =3) was 0.2 μ g/L , and the limit of quantification (LOQ, S/N =10) was 0.6 μ g/L .The recovery of 2,4-diaminotoluene was in the range of 89.0%-94.2%.The relative standard deviations (RSDs) were 1.9%-3.6%.This method requires neither pH adjustment of the soak solution in the pre-processing step nor liquid-liquid extraction.With this method, the pre- processing step is greatly simplified and there is minimal consumption of organic solvents.Further, the method is simple, convenient, and accurate, and it is suitable for the determination of 2,4-diaminotoluene in Mianpi composite packaging film bags.

关 键 词：离子交换固相萃取 气相色谱-质谱联用 2 4-二氨基甲苯 方便面皮复合包装袋 

分 类 号：O658[理学—分析化学]