GC-MS Determinatiom of Residual Amount of Dimethyl Fumarate in Packaging Film and Packaging Bag
摘 要
提出了气相色谱-质谱联用法测定包装膜和包装袋中富马酸二甲酯残留量的方法.样品中富马酸二甲酯用乙酸乙酯萃取,经针式过滤头净化,采用HP-5MS毛细管色谱柱(30 m×0.25 mm,0.25 μm)进行分离.采用气相色谱-质谱电子电离源和全扫描监测模式进行测定.富马酸二甲酯的质量浓度在0.5~100.0 mg·L-1浓度范围与其对应的峰面积呈线性关系,测定下限(10S/N)为0.1 mg·kg-1.在5.0,10.0,20.0,30.0,40.0,50.0 mg·kg-1 6个添加水平下,富马酸二甲酯的回收率在95.0%~102.5%之间,相对标准偏差(n=6)小于6%.
Abstract
Residual amount of dimethyl fumarate in packaging film and packaging bag was determined by GC and MS in hyphenation.The sample was extracted with ethyl acetate,and the dimethyl fumarate in the extract was purified by passing through needle filter head.In the GC-MS analysis,HP-5MS capillary chromatographic column (30 m×0.25 mm,0.25 μm) was used for separation,and modes of electron bombardment ionization ion source (EI) and full scan monitoring were adopted for measurements.Linear relationship between values of peak area and mass concentration of dimethyl fumarate was kept in the range of 0.5-100.0 mg·L-1,and lower limit of determination (10S/N) found was 0.1 mg·kg-1.Test for recovery was made by standard addition method at 6 concentration levels of 5.0,10.0,20.0,30.0,40.0,50.0 mg·kg-1,and the results obtained were in the range of 95.0%-102.5%,with values of RSD′s (n=6) less than 6%.
中图分类号 O657.63
所属栏目 工作简报
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收稿日期 2009/8/17
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备注徐宁(1975-),男,广东汕头人,工程师,主要从事食品化工产品质量分析.
引用该论文: XU-Ning,ZHU Hong,CHEN Xiao-hong. GC-MS Determinatiom of Residual Amount of Dimethyl Fumarate in Packaging Film and Packaging Bag[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(7): 762~764
徐宁,朱虹,陈晓红. 气相色谱-质谱联用法测定包装膜和包装袋中富马酸二甲酯残留量[J]. 理化检验-化学分册, 2010, 46(7): 762~764
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【3】深圳市计量质量检测研究院.2009/251/EC欧盟禁止富马酸二甲酯DMF决议中文全文[EB/OL].http://hi.baidu.com/sz_smq/blog/item/37b998311b38c911ebc4af95.html.2009-4-20.
【4】中国服装在线网.欧盟再颁新指令富马酸二甲酯含量不能超过0.1mg/kg[EB/OL].http://www.fashionline.cn/news/review.asp?articleid=16030&article-classid=94.2009-5-29.
【5】中国国际电子商务网.美国服装鞋业协会公布第四版全球禁用物质清单[EB/OL].http://texquo.ec.com.cn/article/news/200903/728584_1.html.2009-3-13.
【6】国家质量监督检验检疫总局.关于下发轻纺消费品中富马酸二甲酯测定方法试行的通知[EB/OL].http://www.lnciq.gov.cn/zwpd/kjgz/tzgz/200901/t20090105_20967.htm.2009-01-05.
【7】张龙,于宝杰.紫外分光光度法测定富马酸二甲酯的含量[J].石油化工,1999,28(7):477-479.
【8】刘升一,苏柯.高效液相色谱法测定防霉剂富马酸二甲酯[J].色谱,1998,16(2):180-181.
【9】张杨,陈伟强.薄层法检测富马酸二甲酯的含量[J].中国卫生检验杂志,2001,11(6):722-722.
【10】GB/T 6041-2002质谱分析方法通则[S].
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