地质调查样品中有机氯农药分析存在的困难和解决方法
Problems and Solutions in the Determination of Organochlorine Pesticides in Geological Survey Samples
-
摘要: 9种有机氯农药(六氯苯、α-HCH、β-HCH、γ-HCH、δ-HCH、p,p'-DDE、p,p'-DDD、o,p'-DDT和p,p'-DDT)是国土资源地质大调查项目中水和土壤样品必测的有机污染物。有机氯农药自身结构和性质的特殊性以及地质调查样品的差异性,在采用气相色谱电子捕获检测器(GC-ECD)分析有机氯农药过程中仍然存在许多困难。文章结合大量地质调查样品中有机氯农药分析的实践经验,从溶剂与待测物响应值的关系、基质效应的表现、样品前处理以及仪器日常维护四个方面,介绍了针对不同样品和分析要求正确选择进样溶剂、判断和解决基质效应,并通过良好的仪器日常维护习惯确保地质调查样品中有机氯农药检测灵敏度达到要求。Abstract: Nine organochlorine pesticides(HCB, α-HCH, β-HCH, γ-HCH, δ-HCH, p,p'-DDE, p,p'-DDD, o,p'-DDT and p,p'-DDT)in water and soil samples are the priority pollutants to be determined in geological survey project. There are some analytical problems from complex sample matrix and some special properties of these pollutants when gas chromatography with electron capture detector was used. Based on the experiences in analysis of thousands of survey samples, how to diagnose and solve the problems were discussed from following four aspects:1) the relationship between solvent and analyte response, 2) sample matrix effect, 3) sample pretreatment, 4) instrument measurement. These experiences will help analysts to solve the analytical problems and obtain reliable analytical data.
-
Keywords:
- geological /
- survey /
- sample /
- organochlorine /
- pesticides
-
-
Bordajandi L R, Ramos1 J J, Sanz J, González M J, Ramos L.Comprehensive two-dimensional gas chromatography in the screening of persistent organohalogenated pollutants in environmental samples [J].Journal of Chromatography A,2008,1186:312-324. Bordajandi L R, Ramos1 J J, Sanz J, González M J, Ramos L.Comprehensive two-dimensional gas chromatography in the screening of persistent organohalogenated pollutants in environmental samples [J].Journal of Chromatography A,2008,1186:312-324.
Lourencetti C, Navickiene S, Ribeiro M L, Santiago M. Determination of organochlorine pesticides and polychlori-nated biphenyls residues in municipal solid waste compost by gas chromatography with electron capture detection [J]. Chromatographia,2004,59:769-773. Lourencetti C, Navickiene S, Ribeiro M L, Santiago M. Determination of organochlorine pesticides and polychlori-nated biphenyls residues in municipal solid waste compost by gas chromatography with electron capture detection [J]. Chromatographia,2004,59:769-773.
Wang W T, Meng B J, Lu X X, Liu Y, Tao S. Extraction of polycyclic aromatic hydrocarbons and organochlorine pesticides from soils:A comparison between Soxhlet extraction, microwave-assisted extraction and accelerated solvent extraction techniques[J].Analytica Chimica Acta,2007,602:211-222. Wang W T, Meng B J, Lu X X, Liu Y, Tao S. Extraction of polycyclic aromatic hydrocarbons and organochlorine pesticides from soils:A comparison between Soxhlet extraction, microwave-assisted extraction and accelerated solvent extraction techniques[J].Analytica Chimica Acta,2007,602:211-222.
饶竹,李松,吴淑琪,黄毅,王苏明,宋淑玲,谢原利,贾静,田芹. 地质调查中有机物分析方法研究及应用[J]. 地球学报,2009,30 (3):291-300. US EPA Method 8081A.Organochlorine pesticides by gas chromatography[S]. US EPA Method 8081A.Organochlorine pesticides by gas chromatography[S].
US EPA Method 8270C. Semivolatile organic compounds by gas chromatography/mass spectrometry (GC/MS)[S]. US EPA Method 8270C. Semivolatile organic compounds by gas chromatography/mass spectrometry (GC/MS)[S].
Schenck F J, Lehotay S J. Does further clean-up reduce the matrix enhancement effect in gas chromatographic analysis of pesticide residues in food? [J].Journal of Chromatography A,2000,868:51-61. Schenck F J, Lehotay S J. Does further clean-up reduce the matrix enhancement effect in gas chromatographic analysis of pesticide residues in food? [J].Journal of Chromatography A,2000,868:51-61.
李松,饶竹,宋淑玲.全国地下水调查中12种半挥发性必测组分的测定[J].岩矿测试,2008,27(2):91-94. Matovská K, Lehotay S J. Evaluation of common organic solvents for gas chromatographic analysis and stability of multiclass pesticide residues [J].Journal of Chromatography A,2004,1040:259-272. Matovská K, Lehotay S J. Evaluation of common organic solvents for gas chromatographic analysis and stability of multiclass pesticide residues [J].Journal of Chromatography A,2004,1040:259-272.
Benoit F M, Williams D T. Determination of hexachloro-cyclopentadiene at the nanogram per liter level in drinking water [J].Bulletin of Environment Contamination and Toxicology,1981,27(3):303-308. Benoit F M, Williams D T. Determination of hexachloro-cyclopentadiene at the nanogram per liter level in drinking water [J].Bulletin of Environment Contamination and Toxicology,1981,27(3):303-308.
Anastassiades M, Matovsk K, Lehotay S J. Evaluation of analyte protectants to improve gas chromatographic analysis of pesticides [J].Journal of Chromatography A,2003,1015:163-184. Anastassiades M, Matovsk K, Lehotay S J. Evaluation of analyte protectants to improve gas chromatographic analysis of pesticides [J].Journal of Chromatography A,2003,1015:163-184.
宋淑玲,饶竹,胡蔻蔻.进样溶剂极性和汽化室处理方法对有机氯农药灵敏度的影响[J].岩矿测试,2009,28(1):21-24. Erney D R, Gillespie A M, Gilvydis D M, Polle C F. Explanation of the matrix-induced chromatographic response enhancement of organophosphorus pesticides during open tubular column gas chromatography with splitless or hot column injection and flame photometric detection [J].Journal of Chromatographia,638:57-63. Erney D R, Gillespie A M, Gilvydis D M, Polle C F. Explanation of the matrix-induced chromatographic response enhancement of organophosphorus pesticides during open tubular column gas chromatography with splitless or hot column injection and flame photometric detection [J].Journal of Chromatographia,638:57-63.
Hajlov J, Holadov K, Kocourek V, Poustka J, Godula M, Cuhra P, Kempn M. Matrix-induced effects: A critical point in the gas chromatographic analysis of pesticide residues [J].Journal of Chromatography A,1998,800(2):283-295. Hajlov J, Holadov K, Kocourek V, Poustka J, Godula M, Cuhra P, Kempn M. Matrix-induced effects: A critical point in the gas chromatographic analysis of pesticide residues [J].Journal of Chromatography A,1998,800(2):283-295.
Torres M E H, Gonzdlez F J E, Cuadros-Rodrlguez L, Lopez E A, Vidal J L M. Assessment of matrix effects in gas chromatography electron capture pesticide-residue analysis[J].Chromatographia,2003,57:657-664. Torres M E H, Gonzdlez F J E, Cuadros-Rodrlguez L, Lopez E A, Vidal J L M. Assessment of matrix effects in gas chromatography electron capture pesticide-residue analysis[J].Chromatographia,2003,57:657-664.
Schenck F J, Lehotay S J, Victor Vega. Comparison of solid-phase extraction sorbents for cleanup in pesticide residue analysis of fresh fruits and vegetables [J].Journal of Separation Science,2002,25:883-890. Schenck F J, Lehotay S J, Victor Vega. Comparison of solid-phase extraction sorbents for cleanup in pesticide residue analysis of fresh fruits and vegetables [J].Journal of Separation Science,2002,25:883-890.
Stuber M, Reemtsma T. Evaluation of three calibration methods to compensate matrix effects in environmental analysis with LC-ESI-MS [J].Analytical and Bioanalytical Chemistry,2004,378:910-916. Stuber M, Reemtsma T. Evaluation of three calibration methods to compensate matrix effects in environmental analysis with LC-ESI-MS [J].Analytical and Bioanalytical Chemistry,2004,378:910-916.
Bester K, Bordin G, Rodriguez A, Schimmel H, Pauwels J, VanVyncht G. How to overcome matrix effects in the determination of pesticides in fruit by HPLC-ESI-MS-MS [J].Freseniu's Journal of Analy-tical Chemistry,2001,371:550-555. Bester K, Bordin G, Rodriguez A, Schimmel H, Pauwels J, VanVyncht G. How to overcome matrix effects in the determination of pesticides in fruit by HPLC-ESI-MS-MS [J].Freseniu's Journal of Analy-tical Chemistry,2001,371:550-555.
Frenich A G, Martínez Vidal J L, Fernndez Moreno J L, Romero-Gonzlez R. Compensation for matrix effects in gas chromatography tandem mass spectrometry using a single point standard addition [J].Journal of Chromatography A,2009,1216 (23):4798-4808. Frenich A G, Martínez Vidal J L, Fernndez Moreno J L, Romero-Gonzlez R. Compensation for matrix effects in gas chromatography tandem mass spectrometry using a single point standard addition [J].Journal of Chromatography A,2009,1216 (23):4798-4808.
Schantz M M, Parris R M, Kurz J, Ballschmiter K, Wise S A. Comparison of methods for the gas-chromatographic determination of PCB congeners and chlorinated pesticides in marine reference materials [J].Freseniu's Journal of Analytical Chemstry,1993,346:766-778. Schantz M M, Parris R M, Kurz J, Ballschmiter K, Wise S A. Comparison of methods for the gas-chromatographic determination of PCB congeners and chlorinated pesticides in marine reference materials [J].Freseniu's Journal of Analytical Chemstry,1993,346:766-778.
Huang S P, Huang S D. Determination of organochlo-rine pesticides in water using solvent cooling assisted dynamic hollow-fiber-supported headspace liquid-phase microextraction [J].Journal of Chromatography A,2007,1176:19-25. Huang S P, Huang S D. Determination of organochlo-rine pesticides in water using solvent cooling assisted dynamic hollow-fiber-supported headspace liquid-phase microextraction [J].Journal of Chromatography A,2007,1176:19-25.
计量
- 文章访问数: 1764
- HTML全文浏览量: 0
- PDF下载量: 1045