色谱

色谱 ›› 2019, Vol. 37 ›› Issue (10): 1053-1058.DOI: 10.3724/SP.J.1123.2019.01024

• 特别策划：固相萃取和QuEChERS应用专栏 • 上一篇    下一篇

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

芦智远1, 王冰2, 田娜1, 张耀武1, 张新宇1, 刘佳1, 吕岩1   

  1. 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
  • 收稿日期:2019-02-02 出版日期:2019-10-08 发布日期:2020-12-11
  • 通讯作者: 张耀武E-mail:1009693925@qq.com.
  • 基金资助:
    国家粮食局行业标准项目（国粮办发[2017]177号）.

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

LU Zhiyuan1, WANG Bing2, TIAN Na1, ZHANG Yaowu1, ZHANG Xinyu1, LIU Jia1, LÜ Yan1   

  1. 1. Xi'an Supervision & Inspection Institute of Product Quality, Xi'an 710065, China;
    2. Xi'an Institute of Measurement and Testing Technology, Xi'an 710086, China
  • Received:2019-02-02 Online:2019-10-08 Published:2020-12-11
  • Supported by:
    Industry Standard Project of State Administration of Grain (Office[2017]177).

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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5.0 mL水淋洗小柱，用3.0 mL 5%（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1~50 μg/L范围内，线性相关系数（r）为0.9991，检出限（S/N=3）为0.2 μg/L，定量限（S/N=10）为0.6 μg/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。

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

Abstract: 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 μg/L, the linear correlation coefficient (r) was 0.9991. The limit of detection (LOD, S/N=3) was 0.2 μg/L, and the limit of quantification (LOQ, S/N=10) was 0.6 μg/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.

Key words: ion exchange solid phase extraction, gas chromatography-mass spectrometry (GC-MS), 2,4-diaminotoluene, Mianpi composite packaging film bag

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