顶空—气相色谱质谱联用法测定热熔胶中的苯及苯系物
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- 英文论文题名：Determ ination of benzene and its homologues in hot melt adhesives by headspace gas chromatography-mass spectrometry
- 论文作者：张凤梅 ; 司晓喜 ; 朱瑞芝 ; 申钦鹏 ; 刘春波 ; 何沛 ; 王昆淼 ; 杨光宇 ; 苏钟璧 ; 王晋 ; 刘志华
- 英文论文作者：ZHANG Fengmei ; SI Xiaoxi ; ZHU Ruizhi ; SHEN Qinpeng ; LIU Chunbo ; HE Pei ; WANG Kunmiao ; YANG Guangyu ; SU Zhongbi ; WANG Jin ; LIU Zhihua ; R&D Center ; China Tobacco Yunnan Industrial Co. ; Ltd.
- 年：2016
- 作者机构：云南中烟工业有限责任公司技术中心;
- 论文关键词：卷烟 ; 热熔胶 ; 苯 ; 苯系物 ; 顶空—气质联用法
- 英文论文关键词：Cigarette ; Hot melt adhesive ; Benzene ; Benzene homologue ; Headspace gas chromatography-mass spectrometry
- 会议召开时间：2016-12-01
- 会议录名称：中国烟草学会2016年度优秀论文汇编——烟草工业主题
- 语种：中文
- 分类号：TQ436.4;TS42
- 学会代码：ZGYG
- 学会名称：中国烟草学会
- 页数：6
- 文件大小：384k
- 原文格式：D
摘要
为准确测定热熔胶中苯及苯系物的含量,通过对顶空进样条件、气相色谱条件和质谱参数进行考察和优化,建立了一种用顶空一气相色谱质谱联用仪(HS-GC/MS)测定热熔胶中苯及苯系物(苯、甲苯、乙苯、对-二甲苯、间-二甲苯、邻-二甲苯和苯乙烯)的方法,并采用该方法测定了15个热熔胶样品。结果表明:①优化确定的实验条件为,0.20 g剪碎的热熔胶样品,加入1 mL含氘代苯内标(0.10 mg/L)的三乙酸甘油酯(基质校正剂),140 ℃下平衡30 min后顶空进样,采用键合/交联聚乙醇毛细管色谱柱在选择离子监测模式下进行GC/MS分析。②苯及苯系物的检出限在0.01-0.03 mg/kg之间,精密度和回收率分别为1.29%～3.45%和94.1%～99.9%。③15个热熔胶样品中苯及苯系物均有不同程度检出,苯的检出率为13.3%,检出量0.03～0.04 mg/kg;甲苯、乙苯、对-二甲苯、间-二甲苯和邻-二甲苯的检出率均为100%,检出量分别为0.09～3.71、0.15～0.29、0.09～0.29、0.16～0.50和0.15～0.47 mg/kg;苯乙烯检出率86.7%,检出量0.14～0.71 mg/kg。该方法前处理简单、结果准确可靠,适用于热熔胶中苯及苯系物的常规检测。
For accurate quantification of benzene and its homologues(toluene, ethylbenzene,P-xylene, m-xylene,o-xylene and styrene)in hot melt adhesives,a headspace gas chromatography-mass spectrometry(HS.GC/MS)method was established.Experiments were performed to optimize the conditions and parameters of headspace sampling,and GC/M S parameters.Fifteen samples of hot melt adhesives were analyzed with the established method.The results showed that:1 1 The optimized experimental conditions used 0.20 g samples of hot melt adhesives,followed by extraction in 1 m L glyceryl triacetate(matrix correction agent)with deuterated benzene interna1 standard f0.1 0 mg/L)addition.21 The limits of detection for benzene and its homologues were 0.0 1-0.03 mg/kg.The precision of method ranged from 1.29% to 3.45% with the recoveries from 94.1% to 99.9%.3、The levels of benzene and its homologues determined in the 1 5 samples varied.The detection rate of benzene was 1 3.3% with the 1eve1 ranged from 0.03 to 0.04 mg/kg. The detection rates of toluene,ethylbenzene,p-xylene,m-xylene and o-xylene reached 100% with the levels ranged from 0.09 to 3.71,0.15 to 0.29,0.09 t0 0.29,0.16 to 0.50 and 0.15 to 0.47 mg/kg,respectively.The detection rate of styrene was 86.7% with the level ranged from 0.14 to 0.7 1 mg/kg.This method is simple,accurate,reliable and suitable for the routine determination of benzene and its homologues in hot melt adhesives.
For accurate quantification of benzene and its homologues(toluene, ethylbenzene,P-xylene, m-xylene,o-xylene and styrene)in hot melt adhesives,a headspace gas chromatography-mass spectrometry(HS.GC/MS)method was established.Experiments were performed to optimize the conditions and parameters of headspace sampling,and GC/M S parameters.Fifteen samples of hot melt adhesives were analyzed with the established method.The results showed that:1 1 The optimized experimental conditions used 0.20 g samples of hot melt adhesives,followed by extraction in 1 m L glyceryl triacetate(matrix correction agent)with deuterated benzene interna1 standard f0.1 0 mg/L)addition.21 The limits of detection for benzene and its homologues were 0.0 1-0.03 mg/kg.The precision of method ranged from 1.29% to 3.45% with the recoveries from 94.1% to 99.9%.3、The levels of benzene and its homologues determined in the 1 5 samples varied.The detection rate of benzene was 1 3.3% with the 1eve1 ranged from 0.03 to 0.04 mg/kg. The detection rates of toluene,ethylbenzene,p-xylene,m-xylene and o-xylene reached 100% with the levels ranged from 0.09 to 3.71,0.15 to 0.29,0.09 t0 0.29,0.16 to 0.50 and 0.15 to 0.47 mg/kg,respectively.The detection rate of styrene was 86.7% with the level ranged from 0.14 to 0.7 1 mg/kg.This method is simple,accurate,reliable and suitable for the routine determination of benzene and its homologues in hot melt adhesives.
引文
[1]YC/T 187—2004烟用热熔胶[S].YC/T 187—2004 Hot-melt adhesive for cigarette[S].
[2]许真.室内空气主要污染物及其健康效应[J].卫生研究,2003,32(3):279-283.XU Zhen.A main indoor air pollutants and their health impacts[J].Journal of Hygiene Research,2003,32(3):279-283.
[3]孙毓国.室内污染物苯系物危害现状及防治对策[J].北方环境,2012,27(5):234-236.SUN Yuguo.The indoor pollutants BTEX harm situation and control counterasures[J].Northern Environmental,2012,27(5):234-236.
[4]Borgerding M,Klus H.Analysis of complex mixtures—cigarette smoke[J].Experimental and Toxicologic Pathology,2005,57:43-73.
[5]臧志鹏,吕长平,王文婷,等.GC/MS法测定水基胶中苯及苯系物的不确定度[J].烟草科技,2014(7):45-50.ZANG Zhipeng,LU Zhangping,WANG Wenting,et al.Evaluation of uncertainty in determ ination of benzene and its homologues in water-based adhesive by GC/MS [J].Tobacco Science&J Technology,2014(7):45-50.
[6]YC/T 334—2010烟用水基胶苯、甲苯及二甲苯的测定气相色谱-质谱联用法[S].YC/T 334—2010 Determination of benzene.toluene and xylene in water-borne adhesives for cigarette—Gas chromatography-mass spectrometry method[S].
[7]黄宗平,黄长春,潘忠厚,等.顶空气相色谱法同时测定树脂工艺品中7种残留苯系物[J].分析测试学报,2013(5):570-574.HUANG Zongping,HUANG Changchun,PAN Zhonghou,et al.Simultaneous determ ination of 7residual benzene series in resin crafts by headspace gas chromatography [J].Journal of Instrumental Analysis,2013(5):570-574.
[8]穆小丽,梅丹丹,欧舟,等.气相色谱-质谱选择性测定三乙酸甘油酯中的苯系物[J].湖南师范大学自然科学学报,2015(3):40-44.MU Xiaoli,MEl Dandan.OU Zhou.et al.Selective determ ination of benzene series com ponents in triacetin by gas chromatography-mass spectrometry[J].Journal of Natural Science of Hunan Normal University,2015(3):40-44.
[9]侯宏卫,熊巍,姜兴益,等.气相色谱-质谱联用法测定卷烟主流烟气气相物中挥发性有机化合物[J].中国烟草科学,2011,32(5):81-86.HOU Hongwei,XIONG Wei,JIANG Xingyi,et al.Determination of volatile organic com pounds in gas-phase mainstream sm oke by gas chrom atography-mass spectrometry [J].Chinese Tobacco Science,2011,32(5):81-86.
[10]韩冰,王海艳.冷溶剂-气相色谱/质谱联用分析卷烟主流烟气气相成分[J].广东化工,2011,38(7):148-150.HAN Bing,W ANG Haiyan.Analysis of com ponents in mainstream cigarette smoke by cryogenic trap and gas chromatography/mass spectrometry[J].Guangdong Chemical Industry,201l,38(7):148-150.
[11]韩冰,蔡君兰,王冰,等.部分国内外卷烟主流烟气气相和粒相中挥发性、半挥发性化合物的分析[J].中国烟草学报,2011,17(4):1-7.HAN Bing,CAI Junlan,WANG Bing,et al.Analysis of volatile and semi-volatile components in both gas and particulate phase mainstream cigarette sm oke with domestic and foreign made cigarette[J].Acta Tabacaria Sinica,2011,17(4):1-7.
[12]韩冰,刘惠民,谢复炜,等.卷烟主流烟气中挥发和半挥发性成分分析[J].炯草科技,2009(10):32-40.HAN Bing,LIU Huim in,XIE Fuwei,et al.Analysis of volatile and semi-volatile components in mainstream cigarette smoke [J].Tobacco Science&Technology,2009(10):32-40.
[13]刘剑,姬厚伟,韩伟,等.冷阱捕集-气相色谱-质谱法测定卷烟主流炯气气相物中的苯系物[J].烟草科技,2014(4):74-78.LIU Jian,JI Houwei.HAN Wei,et al.Determ ination of benzene hom ologues in gas phase of m ainstream cigarette smoke by cold trap and gas chromatography-mass spectrometry [J].Tobacco Science&Technology,2014(4):74-78.
[14]YC/T 373-20l0丙纤丝束及丙纤滤棒苯、甲笨、乙苯和二甲苯残留量的测定气相色谱法[s].YC/T 373-20l0 Determ ination of benzene.toluene ethylbenzene and xylene in polypropylene fiber tow and polypropylene fiber tow filter rod-Gas chrom atography-mass spectrometry method [s].
[15]李中皓,李雪,王庆华,等.顾空-气质联用内标法检测印刷油墨中的苯及苯系物[J].现代食品科技,2011,27(5):587-590.LI Zhonghao,LI Xue,WANG Qinghua,et al.Determ ination of benzene,toluene,ethylbenzene and xylene(BTEX)in printing ink by headspace-GC/MS with internal standard [J].Modem Food Science and Technology,2011.27(5):587-590.
[16]李中皓,唐纲岭,陈再根,等.顶空-气质联用法测定卷烟包装材料中苯不确定度评定[J].质谱学报,2009,30(6):359-363.LI Zhonghao,TANG Gangling,CHEN Zaigen,et al.Evaluation of uncertainty of volatile benzene in cigarette packing material by HS-GC/MS[J].Journal of Chinese Mass Spectrometry Society,2009,30(6):359-363.
[17]姬厚伟,满杰,刘剑,等.静态顶空GC/MS测定卷烟滤嘴截留的烟气中苯系物[J].中国烟草学报,2015,21(2):23-28.JI Houwei,MAN Jie,LIU Jian,et al.Determ ination of benzene compounds in m ainstream cigarette smoke entrapped by filter using static headspace GC/M S method[J].Acta Tabacaria Sinica,2015,21(2):23-28.
[2]许真.室内空气主要污染物及其健康效应[J].卫生研究,2003,32(3):279-283.XU Zhen.A main indoor air pollutants and their health impacts[J].Journal of Hygiene Research,2003,32(3):279-283.
[3]孙毓国.室内污染物苯系物危害现状及防治对策[J].北方环境,2012,27(5):234-236.SUN Yuguo.The indoor pollutants BTEX harm situation and control counterasures[J].Northern Environmental,2012,27(5):234-236.
[4]Borgerding M,Klus H.Analysis of complex mixtures—cigarette smoke[J].Experimental and Toxicologic Pathology,2005,57:43-73.
[5]臧志鹏,吕长平,王文婷,等.GC/MS法测定水基胶中苯及苯系物的不确定度[J].烟草科技,2014(7):45-50.ZANG Zhipeng,LU Zhangping,WANG Wenting,et al.Evaluation of uncertainty in determ ination of benzene and its homologues in water-based adhesive by GC/MS [J].Tobacco Science&J Technology,2014(7):45-50.
[6]YC/T 334—2010烟用水基胶苯、甲苯及二甲苯的测定气相色谱-质谱联用法[S].YC/T 334—2010 Determination of benzene.toluene and xylene in water-borne adhesives for cigarette—Gas chromatography-mass spectrometry method[S].
[7]黄宗平,黄长春,潘忠厚,等.顶空气相色谱法同时测定树脂工艺品中7种残留苯系物[J].分析测试学报,2013(5):570-574.HUANG Zongping,HUANG Changchun,PAN Zhonghou,et al.Simultaneous determ ination of 7residual benzene series in resin crafts by headspace gas chromatography [J].Journal of Instrumental Analysis,2013(5):570-574.
[8]穆小丽,梅丹丹,欧舟,等.气相色谱-质谱选择性测定三乙酸甘油酯中的苯系物[J].湖南师范大学自然科学学报,2015(3):40-44.MU Xiaoli,MEl Dandan.OU Zhou.et al.Selective determ ination of benzene series com ponents in triacetin by gas chromatography-mass spectrometry[J].Journal of Natural Science of Hunan Normal University,2015(3):40-44.
[9]侯宏卫,熊巍,姜兴益,等.气相色谱-质谱联用法测定卷烟主流烟气气相物中挥发性有机化合物[J].中国烟草科学,2011,32(5):81-86.HOU Hongwei,XIONG Wei,JIANG Xingyi,et al.Determination of volatile organic com pounds in gas-phase mainstream sm oke by gas chrom atography-mass spectrometry [J].Chinese Tobacco Science,2011,32(5):81-86.
[10]韩冰,王海艳.冷溶剂-气相色谱/质谱联用分析卷烟主流烟气气相成分[J].广东化工,2011,38(7):148-150.HAN Bing,W ANG Haiyan.Analysis of com ponents in mainstream cigarette smoke by cryogenic trap and gas chromatography/mass spectrometry[J].Guangdong Chemical Industry,201l,38(7):148-150.
[11]韩冰,蔡君兰,王冰,等.部分国内外卷烟主流烟气气相和粒相中挥发性、半挥发性化合物的分析[J].中国烟草学报,2011,17(4):1-7.HAN Bing,CAI Junlan,WANG Bing,et al.Analysis of volatile and semi-volatile components in both gas and particulate phase mainstream cigarette sm oke with domestic and foreign made cigarette[J].Acta Tabacaria Sinica,2011,17(4):1-7.
[12]韩冰,刘惠民,谢复炜,等.卷烟主流烟气中挥发和半挥发性成分分析[J].炯草科技,2009(10):32-40.HAN Bing,LIU Huim in,XIE Fuwei,et al.Analysis of volatile and semi-volatile components in mainstream cigarette smoke [J].Tobacco Science&Technology,2009(10):32-40.
[13]刘剑,姬厚伟,韩伟,等.冷阱捕集-气相色谱-质谱法测定卷烟主流炯气气相物中的苯系物[J].烟草科技,2014(4):74-78.LIU Jian,JI Houwei.HAN Wei,et al.Determ ination of benzene hom ologues in gas phase of m ainstream cigarette smoke by cold trap and gas chromatography-mass spectrometry [J].Tobacco Science&Technology,2014(4):74-78.
[14]YC/T 373-20l0丙纤丝束及丙纤滤棒苯、甲笨、乙苯和二甲苯残留量的测定气相色谱法[s].YC/T 373-20l0 Determ ination of benzene.toluene ethylbenzene and xylene in polypropylene fiber tow and polypropylene fiber tow filter rod-Gas chrom atography-mass spectrometry method [s].
[15]李中皓,李雪,王庆华,等.顾空-气质联用内标法检测印刷油墨中的苯及苯系物[J].现代食品科技,2011,27(5):587-590.LI Zhonghao,LI Xue,WANG Qinghua,et al.Determ ination of benzene,toluene,ethylbenzene and xylene(BTEX)in printing ink by headspace-GC/MS with internal standard [J].Modem Food Science and Technology,2011.27(5):587-590.
[16]李中皓,唐纲岭,陈再根,等.顶空-气质联用法测定卷烟包装材料中苯不确定度评定[J].质谱学报,2009,30(6):359-363.LI Zhonghao,TANG Gangling,CHEN Zaigen,et al.Evaluation of uncertainty of volatile benzene in cigarette packing material by HS-GC/MS[J].Journal of Chinese Mass Spectrometry Society,2009,30(6):359-363.
[17]姬厚伟,满杰,刘剑,等.静态顶空GC/MS测定卷烟滤嘴截留的烟气中苯系物[J].中国烟草学报,2015,21(2):23-28.JI Houwei,MAN Jie,LIU Jian,et al.Determ ination of benzene compounds in m ainstream cigarette smoke entrapped by filter using static headspace GC/M S method[J].Acta Tabacaria Sinica,2015,21(2):23-28.
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