便携式气相色谱-质谱法测定工作场所空气中2-甲基丙醛、2-甲基丁醛和3-甲基丁醛
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摘要
目的建立便携式气相色谱-质谱(GC-MS)法测定工作场所空气中2-甲基丙醛、2-甲基丁醛和3-甲基丁醛的方法。方法利用便携式GC-MS仪取样探头直接采集工作场所空气,经Tri-bed吸附管富集后,热解吸进样分析,采用保留时间和特征离子定性,特征离子峰面积定量。结果本方法检测2-甲基丙醛、2-甲基丁醛、3-甲基丁醛的线性范围分别为0. 079～15. 880、0. 080～16. 080、0. 160～32. 120 mg/m~3,相关系数均大于0. 999,检出限分别为0. 012、0. 007、0. 013 mg/m~3,定量下限分别为0. 041、0. 023、0. 044 mg/m~3,加标回收率为92. 2%～104. 4%,批内相对标准偏差(RSD)为5. 8%～9. 1%,批间RSD为9. 3%～19. 6%。结论本方法准确度和精密度较高,适用于工作场所空气中2-甲基丙醛、2-甲基丁醛、3-甲基丁醛的快速定性和定量检测。
Objective To establish a method for detection of 2-methylpropanal,2-methyl butanal and 3-methyl butanal in workplace air by portable gas chromatography-mass spectrometry( GC-MS). Methods The workplace air was collected by portable GC-MS sampling probe. After enrichment by Tri-bed tube,the thermal desorption sample was analyzed by retention time and characteristic ion characterization. The characteristic ion peak area was quantified. Results The linear ranges of 2-methylpropanal,2-methyl butanal and 3-methyl butanal were 0. 079-15. 880,0. 080-16. 080 and 0. 161-32. 120 mg/m~3,respectively. All the correlation coefficients were greater than 0. 999. The detection limits were 0. 012,0. 007 and0. 013 mg/m~3,and the quantitation limits were 0. 041,0. 023 and 0. 044 mg/m~3,respectively. The recovery rates of2-methylpropanal,2-methyl butanal and 3-methyl butanal were 92. 2%-104. 4%. The within-run relative standard deviation( RSD) was 5. 8%-9. 1%. The between-run RSD of different batches samples was 9. 3%-19. 6%. Conclusion This method has high accuracy and is precise,which is suitable for rapid qualitative and quantitative detection of2-methylpropanal,2-methyl butanal and 3-methyl butanal in workplace air.
Objective To establish a method for detection of 2-methylpropanal,2-methyl butanal and 3-methyl butanal in workplace air by portable gas chromatography-mass spectrometry( GC-MS). Methods The workplace air was collected by portable GC-MS sampling probe. After enrichment by Tri-bed tube,the thermal desorption sample was analyzed by retention time and characteristic ion characterization. The characteristic ion peak area was quantified. Results The linear ranges of 2-methylpropanal,2-methyl butanal and 3-methyl butanal were 0. 079-15. 880,0. 080-16. 080 and 0. 161-32. 120 mg/m~3,respectively. All the correlation coefficients were greater than 0. 999. The detection limits were 0. 012,0. 007 and0. 013 mg/m~3,and the quantitation limits were 0. 041,0. 023 and 0. 044 mg/m~3,respectively. The recovery rates of2-methylpropanal,2-methyl butanal and 3-methyl butanal were 92. 2%-104. 4%. The within-run relative standard deviation( RSD) was 5. 8%-9. 1%. The between-run RSD of different batches samples was 9. 3%-19. 6%. Conclusion This method has high accuracy and is precise,which is suitable for rapid qualitative and quantitative detection of2-methylpropanal,2-methyl butanal and 3-methyl butanal in workplace air.
引文
[1]李云辉,李治水,聂增来,等.丁醛异构物塔产品结构的优化研究[J].天津科技,2015,42(11):29-31.
[2]张之翔,曾永康,黄琼淋,等.异丁烯氢甲酰化合成异戊醛的研究[J].应用化工,2018,47(3):486-489,493.
[3]李文,陈万超,杨焱,等.香菇生长过程中挥发性风味成分组成及其风味评价[J].核农学报,2018,32(2):325-334.
[4]沙坤,张泽俊,张松山,等.不同类型新疆风干牛肉挥发性风味成分差异分析[J].肉类研究,2018,32(4):33-38.
[5]乔凯娜,王琳涵,孔琰,等.不同压力下猪肉香精挥发性风味成分的差异性[J].精细化工,2018,35(7):1188-1195.
[6]中华人民共和国卫生部.工作场所有害因素职业接触限值第1部分:化学有害因素:GBZ 2.1-2007[S].北京:人民卫生出版社,2007.
[7]中华人民共和国国家卫生和计划生育委员会.工作场所空气有毒物质测定第99部分:甲醛、乙醛和丁醛:GBZ/T 300.99-2017[S].北京:人民卫生出版社,2017.
[8]范智超,王斐,和莹,等.环境空气中多种羰基化合物的测定[J].环境监测管理与技术,2018,30(2):43-45.
[9]WOLFGANG R,BIBIANA B,RENATE W.Airborne aldehydes in cabin-air of commercial aircraft:Measurement by HPLC with UVabsorbance detection of 2,4-dinitrophenylhydrazones[J].J Chromatogr B,2016,1019:117-127.
[10]中华人民共和国环境保护部行业标准.车内挥发性有机物和醛酮类物质采样测定方法:HJ/T 400-2007[S].北京:中国环境科学出版社,2008.
[11]United States Enivronmental Protection Agency.Compendium of methods for the determination of toxic organic compounds in ambient air compendium method to-11a:determination of formaldehyde in ambient air using adsorbent cartridge followed by high performance liquid chromatography(HPLC)[EB/OL].(1999-01)[2019-05-27].https://www3.epa.gov/ttn/amtic/files/ambient/airtox/to-11ar.pdf.
[12]ZHAO Y,LIU M.The method study on emergency detection of aromatic compounds and chlorides based on portable GC-MS[J].Procedia Eng,2014,84:731-735.
[13]朱海豹,苏成君,唐红芳,等.便携式气相色谱-质谱法快速测定环境空气中的痕量挥发性有机物[J].卫生研究,2017,46(6):981-985.
[14]王瑶,潘兴富,闫慧芳.便携式气相色谱-质谱法测定工作场所空气中三氯乙烯[J].中国职业医学,2014,41(3):339-340,343.
[15]孙冉,闫慧芳.便携式气相色谱-质谱法检测工作场所空气中双氯甲醚[J].中国职业医学,2017,44(4):466-468.
[16]NAGATA Y.Measurement of odor threshold value review of“Measurement of threshold value by tiriangle odor bag method Bull.Jap.Env.Sanit.Cent.No.17.1990”paper[J].J Japan Assoc Odor Environ,2012,43(6):401-407.
[17]颜鲁春,刘杰民,付慧婷,等.异味混合物中组分浓度与其强度贡献关系研究[J].环境科学,2013,34(12):4743-4746.
[2]张之翔,曾永康,黄琼淋,等.异丁烯氢甲酰化合成异戊醛的研究[J].应用化工,2018,47(3):486-489,493.
[3]李文,陈万超,杨焱,等.香菇生长过程中挥发性风味成分组成及其风味评价[J].核农学报,2018,32(2):325-334.
[4]沙坤,张泽俊,张松山,等.不同类型新疆风干牛肉挥发性风味成分差异分析[J].肉类研究,2018,32(4):33-38.
[5]乔凯娜,王琳涵,孔琰,等.不同压力下猪肉香精挥发性风味成分的差异性[J].精细化工,2018,35(7):1188-1195.
[6]中华人民共和国卫生部.工作场所有害因素职业接触限值第1部分:化学有害因素:GBZ 2.1-2007[S].北京:人民卫生出版社,2007.
[7]中华人民共和国国家卫生和计划生育委员会.工作场所空气有毒物质测定第99部分:甲醛、乙醛和丁醛:GBZ/T 300.99-2017[S].北京:人民卫生出版社,2017.
[8]范智超,王斐,和莹,等.环境空气中多种羰基化合物的测定[J].环境监测管理与技术,2018,30(2):43-45.
[9]WOLFGANG R,BIBIANA B,RENATE W.Airborne aldehydes in cabin-air of commercial aircraft:Measurement by HPLC with UVabsorbance detection of 2,4-dinitrophenylhydrazones[J].J Chromatogr B,2016,1019:117-127.
[10]中华人民共和国环境保护部行业标准.车内挥发性有机物和醛酮类物质采样测定方法:HJ/T 400-2007[S].北京:中国环境科学出版社,2008.
[11]United States Enivronmental Protection Agency.Compendium of methods for the determination of toxic organic compounds in ambient air compendium method to-11a:determination of formaldehyde in ambient air using adsorbent cartridge followed by high performance liquid chromatography(HPLC)[EB/OL].(1999-01)[2019-05-27].https://www3.epa.gov/ttn/amtic/files/ambient/airtox/to-11ar.pdf.
[12]ZHAO Y,LIU M.The method study on emergency detection of aromatic compounds and chlorides based on portable GC-MS[J].Procedia Eng,2014,84:731-735.
[13]朱海豹,苏成君,唐红芳,等.便携式气相色谱-质谱法快速测定环境空气中的痕量挥发性有机物[J].卫生研究,2017,46(6):981-985.
[14]王瑶,潘兴富,闫慧芳.便携式气相色谱-质谱法测定工作场所空气中三氯乙烯[J].中国职业医学,2014,41(3):339-340,343.
[15]孙冉,闫慧芳.便携式气相色谱-质谱法检测工作场所空气中双氯甲醚[J].中国职业医学,2017,44(4):466-468.
[16]NAGATA Y.Measurement of odor threshold value review of“Measurement of threshold value by tiriangle odor bag method Bull.Jap.Env.Sanit.Cent.No.17.1990”paper[J].J Japan Assoc Odor Environ,2012,43(6):401-407.
[17]颜鲁春,刘杰民,付慧婷,等.异味混合物中组分浓度与其强度贡献关系研究[J].环境科学,2013,34(12):4743-4746.
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