层析净化-气相色谱-质谱法测定大气颗粒物中7种有机磷酸酯阻燃剂
GC-MS Determination of 7 Organic Phosphate Ester Flame Retardants in Atmospheric Particulates with Chromatography Purification
摘 要
采用层析净化-气相色谱-质谱法测定大气颗粒物中7种有机磷酸酯阻燃剂的含量.大气颗粒物样品经乙酸乙酯-丙酮(3+2)溶液提取,硅胶∶氧化铝(3∶1)层析柱分离纯化.以RTI-5MS色谱柱为固定相,在质谱分析中采用选择离子监测模式.7种有机磷酸酯阻燃剂在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在1.01~8.74 pg·m-3之间.加标回收率在51.9%~89.3%之间,测定值的相对标准偏差(n=3)在3.2%~11%之间.
有机磷酸酯阻燃剂
大气颗粒物
层析净化
GC-MS
Organic phosphate ester flame retardant
Atmospheric particulates
Chromatography purification
Abstract
GC-MS was applied to the determination of 7 organic phosphate ester flame retardants in atmospheric particulates with chromatography purification.The sample of atmospheric particulates was extracted with ethyl acetate-acetone (3+2) solution,and purified with silica∶alumina (3∶1) column chromatography.The RTI-5MS chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS determination.Linear relationships between values of peak area and mass concentration of the 7 organic phosphate ester flame retardants were kept in definite ranges,with detection limits (3S/N) in the range of 1.01-8.74 pg·m-3.Values of recovery found by standard addition method were in the range of 51.9%-89.3%,and values of RSD′s (n=3) in the range of 3.2%-11%.
中图分类号 O657.63
所属栏目 试验与研究
基金项目 国家自然科学青年基金(21407014);四川省科技支撑计划项目(2015GZ0240);校中青年学术带头人科研基金(J201415)
收稿日期 2014/5/28
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备注李世平(1990-),男,湖南益阳人,硕士研究生,主要研究方向为环境污染与监测.
引用该论文: LI Shi-ping,YIN Hong-ling,YE Zhi-xiang,LIANG Jin-feng,HAO Yan-fen. GC-MS Determination of 7 Organic Phosphate Ester Flame Retardants in Atmospheric Particulates with Chromatography Purification[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(5): 581～585
李世平,印红玲,叶芝祥,梁金凤,郝艳芬. 层析净化-气相色谱-质谱法测定大气颗粒物中7种有机磷酸酯阻燃剂[J]. 理化检验－化学分册, 2015, 51(5): 581～585
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【6】FRIES E,MIHAJLOVIC I.Pollution of soils with organophosphorus flame retardants and plasticizers[J].Journal of Environmental Monitoring,2011,13(10):2692-2694.
【7】IVANA M,VOJINOVIC M M,ELKE F.Application of Twisselmann extraction,SPME,and GC-MS to assess input sources for organophosphate esters into soil[J].Environmental Science and Technology,2011,45(6):2264-2269.
【8】GORGA M,PETROVIC M,BARCEL D.Multi-residue analytical method for the determination of endocrine disruptors and related compounds in river and waste water using dual column liquid chromatography switching system coupled to mass spectrometry[J].Journal of Chromatography a,2013,1259:57-66.
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【11】KIM J,ISOBE T,SUDARYANTO A,et al.Organophosphorus flame retardants in house dust from the Philippines: occurrence and assessment of human exposure[J].Environmental Science and Pollution Research,2013,20(2):812-822.
【12】M LLER A,STURM R,XIE Z Y,et al.Organophosphorus flame retardants and plasticizers in airborne particles over the Northern Pacific and Indian Ocean toward the polar regions: evidence for global occurrence[J].Environmental Science and Technology,2012,46(6):3127-3134.
【13】QUINTANA J B,RODIL R,REEMTSMA T,et al.Organophosphorus flame retardants and plasticizers in water and air II.Analytical methodology[J].TRAC Trends in Analytical Chemistry,2008,27(10):904-915.
【14】王成云,李丽霞,谢堂堂,等.超声萃取/气相色谱-串联质谱法同时测定纺织品中6种禁用有机磷阻燃剂[J].分析测试学报,2011,30(8):917-921.
【15】曾铭,蒋小良,苏小东,等.微波辅助萃取-气相色谱-质谱法测定玩具中3种有机磷阻燃剂[J].理化检验-化学分册,2013,49(10):1254-1256.
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