顶空-气相色谱-质谱法测定皂、粉、液类洗涤用品中的二噁烷
Determination of 1,4-Dioxane in Soap, Powder and Liquid Detergents by Headspace-GC-MS
摘 要
提出了测定皂、粉、液类洗涤用品中二噁烷含量的顶空-气相色谱-质谱法。以5 mL水为顶空溶剂,将样品在80 ℃顶空平衡50 min后,经HP-5MS色谱柱分离,质谱检测器检测,外标法定量。3种基质中二噁烷的线性范围为0.1~50.0 mg·kg-1,测定下限均在0.2 mg·kg-1以下。以空白样品为基体进行加标回收实验,测得平均回收率在85.2%~97.8%之间,测定值的相对标准偏差(n=6)在2.6%~6.1%之间。
二噁烷
洗涤用品
Headspace-GC-MS
1,4-Dioxane
Detergents
Abstract
A method of headspace-gas chromatography-mass spectrometry (HS-GC-MS) was applied to the determination of 1,4-dioxane in soap, powder or liquid detergents. The sample was equilibrated at 80 ℃ for 50 min with 5 mL of water as the headspace solvent, then the analyte was separated on HP-5MS column and finally determined by MS. External standard method was adopted for quantification. Linearity ranges of 1,4-dioxane obtained in 3 kinds of detergents were same between 0.1-50.0 mg·kg-1 and lower limits of determination were all less than 0.2 mg·kg-1. Values of recovery found by standard addition method were in the range of 85.2%-97.8% and RSD′s (n=6) were in the range of 2.6%-6.1%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201509022
所属栏目 工作简报
基金项目 质检公益性行业科研专项基金项目(2012104013-9)
收稿日期 2014/7/10
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备注吕庆(1984-),男,河北保定人,工程师,主要从事 日用消费品安全分析。
引用该论文: LV Qing,WANG Zhi-juan,ZHANG Qing,LI Hai-yu,GUO Xiang-yu,BAI Hua. Determination of 1,4-Dioxane in Soap, Powder and Liquid Detergents by Headspace-GC-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(9): 1298～1301
吕庆,王志娟,张庆,李海玉,郭项雨,白桦. 顶空-气相色谱-质谱法测定皂、粉、液类洗涤用品中的二噁烷[J]. 理化检验－化学分册, 2015, 51(9): 1298～1301
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参考文献
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<分析试验室|2008|27|增2|289-292
参考文献原文>崔进,杨佳玲,刘祥.顶空-气相色谱-串联质谱法测定合成洗涤剂及化妆品中二噁烷残留［J］.分析测试学报, 2012,31(11):1446-1450.
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【7】常宇文,田野,曹红.1,4-二噁烷含量测定中固相微萃取头的选择研究［J］.分析测试学报, 200,27(增1):130-133.
【8】贾静,杨志鹏.吹扫捕集-气相色谱-质谱法测定地下水中1,4-二噁烷［J］.岩矿测试, 2014,33(4):556-560.
【9】何松涛,乙小娟,刘一军.进出口酒精中二噁烷的GC-MS检验方法［J］.分析测试学报, 2005,24(增1):315-318.
【10】GB/T 26388-2011 表面活性剂中二噁烷残留量的测定［S］.
【2】田野,常宇文,曹红.食品用洗涤剂中1,4-二噁烷含量检测研究进展［J］.分析试验室, 2008,27(增2):289-292.
<
参考文献原文>崔进,杨佳玲,刘祥.顶空-气相色谱-串联质谱法测定合成洗涤剂及化妆品中二噁烷残留［J］.分析测试学报, 2012,31(11):1446-1450.
【3】中华人民共和国卫生部.化妆品卫生规范［M］.北京:中华人民共和国卫生部, 2007:3-20.
【4】Regulation(EC)No l 223/2009 of the European Parliament and of the Council of 30 November 2009 on Cosmetic Products. Official Journal of the European Union. ［2009-l2-22］. http: //eur-lex. europa. eu/LexUriServ/LexUriServ. do?uri=OJ: L: 2009: 342: 0059: 0209: EN: PDF.
【5】王超,王星,季美琴.GC和GC-MS法测定洗涤及化妆用品中二噁烷残留量［J］.质谱学报, 2005,26(4):254-256.
【6】李晶瑞,马强,李文涛.同位素稀释-顶空气相色谱-质谱联用法测定化妆品中的二噁烷残留量［J］.色谱, 2013,31(5):481-484.
【7】常宇文,田野,曹红.1,4-二噁烷含量测定中固相微萃取头的选择研究［J］.分析测试学报, 200,27(增1):130-133.
【8】贾静,杨志鹏.吹扫捕集-气相色谱-质谱法测定地下水中1,4-二噁烷［J］.岩矿测试, 2014,33(4):556-560.
【9】何松涛,乙小娟,刘一军.进出口酒精中二噁烷的GC-MS检验方法［J］.分析测试学报, 2005,24(增1):315-318.
【10】GB/T 26388-2011 表面活性剂中二噁烷残留量的测定［S］.
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