司晓喜,刘志华,朱瑞芝,申钦鹏,吴亿群,杨光宇,张凤梅.溶剂萃取/气相色谱-质谱法测定热熔胶中苯系物[J].包装工程,2017,38(7):92-96.
SI Xiao-xi,LIU Zhi-hua,ZHU Rui-zhi,SHEN Qin-peng,WU Yi-qun,YANG Guang-yu,ZHANG Feng-mei.Determination of Benzene Series in Hot Melt Adhesives by Solvent Extraction/Gas Chromatography-Mass Spectrometry[J].Packaging Engineering,2017,38(7):92-96. |
| 溶剂萃取/气相色谱-质谱法测定热熔胶中苯系物 |
| Determination of Benzene Series in Hot Melt Adhesives by Solvent Extraction/Gas Chromatography-Mass Spectrometry |
| 投稿时间：2016-08-02 修订日期：2017-04-10 |
| DOI： |
| 中文关键词: 热熔胶 苯系物 残留量 气相色谱-质谱联用法 溶剂萃取 |
| 英文关键词: hot melt adhesives benzene series residues gas chromatography-mass spectrometry solvent extraction |
| 基金项目:中国烟草总公司标准预研项目（2013QB015）；中国烟草总公司标准项目（2013QB008）；云南中烟工业有限责任公司科技开发项目（2015JC06） |
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| 中文摘要: |
| 目的 建立一种溶剂萃取/气相色谱-质谱联用法测定热熔胶中苯系物残留量的方法。方法 优化溶剂萃取条件和仪器分析条件，热熔胶样品依次经超声萃取、冷冻离心后，萃取液通过气相色谱-质谱联用法测定并得到热熔胶中苯系物的残留量，并与顶空-气相色谱/质谱法测定结果进行比较。结果 采用文中方法测定了6种苯系物的线性相关系数大于0.9992，定量限为0.03～0.07 mg/kg，回收率为89.1%～103.1 %。文中方法与顶空进样法对实际样品的测定结果一致，并利用文中方法对70个市售热熔胶样品进行了测定，苯检出率为4.3%，残留量低于0.18 mg/kg，甲苯、乙苯、对-二甲苯、间-二甲苯、邻-二甲苯检出率大于92.9%，其残留量在0.10～58.68 mg/kg。结论 文中方法具有简单、快速、准确度高等优点，适用于热熔胶中苯系物残留量的测定。 |
| 英文摘要: |
| The work aims to determine the benzene series residues in hot melt adhesives by establishing a method of solvent extraction/gas chromatography-mass spectrometry (GC-MS). The conditions of solvent extraction and instrumental analysis were optimized. The hot melt adhesive samples were treated by ultrasonic extraction and refrigerated centrifugation in turn. Then the extract was determined with GC-MS to acquire the content of benzene series residues in hot melt adhesives. The detection results were also compared with those obtained by head space-gas chromatography/mass spectrometry (HS-GC/MS). The linear correlation coefficients of 6 benzene series were determined in the proposed method and they were greater than 0.9992; the limits of quantitation (LOQs) were in the range of 0.03～0.07 mg/kg, and the recovery rate was in the range of 89.1%～103.1%. The results of the actual samples determined in the proposed method were well in agreement with those determined in the headspace sampling method. 70 commercially available hot melt adhesive samples were determined in the proposed method. The determination results showed that the benzene residue was lower than 0.18 mg/kg with detection rate of 4.3%, and the residues of toluene, ethylbenzene, p-xylene, m-xylene and o-xylene ranged from 0.10 mg/kg to 58.68 mg/kg with detection rate higher than 92.9%. The proposed method is characterized by simplicity, rapidness and high accuracy, etc. and it is applicable to the determination of benzene series residues in hot melt adhesives. |
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