Study on carbamate pesticides by capillary electrophoresis with laser-induced fluorescence detection
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摘要: 用毛细管电泳激光诱导荧光检测法(CE-LIF),对灭除威(XMC)、混杀威(2, 3, 5-trimethacarb)和灭虫威(mercaptodimethur)等3种氨基甲酸酯类农药进行了研究.在碱性条件下,氨基甲酸酯类农药水解产生甲胺并与荧光衍生试剂4-氯-7-硝基-2,1,3-苯并二唑(NBD-Cl)发生衍生化反应,产物经毛细管电泳激光诱导荧光检测法测定.对影响水解、衍生以及毛细电泳分离的因素如缓冲液酸度、浓度和衍生试剂的浓度等进行了详细讨论;在最佳条件下,3种农药的检出限分别可达3.010-9、1.010-9和3.010-9 mol/L,并测定了它们的水解速率常数及活化能.该方法不仅可对氨基甲酸酯类农药进行测定,同时也可用于对这类农药的一些理化常数的测定.Abstract: A sensitive and rapid capillary electrophoresis method with laser-induced fluorescence detection (CE-LIF) was developed for the determination of carbamate pesticides (including (3,5-dimethylphenyl) N-methylcarbamate (XMC), and mercaptodimethur). In alkaline solution, carbamate was hydrolyzed to methylamine, which can be derivatized by 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) and detected by CE-LIF. Several parameters which influence the hydrolysis, derivatization and electrophoresis separation, such as pH, concentration of buffer solution and concentration of NBD-Cl, were investigated. The detection limits of the three carbamates were 3.010-9、1.010-9 and 3.010-9 mol/L, respectively. The proposed method was successfully employed to determine the rate constants and activation energies for carbamates hydrolysis.
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[1] [1] DUGAY J, MIEGE C, HENNION M C. Effect of the various parameters governing solid-phase microextraction for the trace-determination of pesticides in water[J]. Journal of Chromatography A, 1998, 795(1): 27-42.[2] OKUMURA T, IMAMURA K, NISHIKAWA Y, et al. Determination of carbamate pesticides in environmental samples as their trifluoroacetyl or methyl derivatives by using gas chromatography-mass spectrometry[J]. Analyst, 1995, 120(11): 2675-81.[3] SAITO T, YAMASHITA O, MIYATA T. Critical review of endocrine disrupters in applied entomology[J]. Ja- panese Journal of Applied Entomology and Zoology, 2000,44(3): 115-164. [4] US Environmental Protection Agency. National Survey of Pesticides in Drinking Water Wells, Phase Ⅱ Report, EPA 570/9-91-020[R]. Springfield, VA: National Technical Information Service, 1992.[5] PAíGA P, MORAIS S, CORREIA M, et al. Determination of carbamate and urea pesticide residues in fresh vegetables using microwave-assisted extraction and liquid chromatography[J]. International Journal of Environmental Analytical Chemistry, 2009, 89(3): 199-210.[6] 刘丽萍.高效液相色谱柱后衍生法测定蔬菜中氨基杀虫剂农药残留[J].中国实用医药,2008, 3(8):116.[7] SABALA A, PORTILLO J L, BROTO-PUIG F, et al. Development of a new high-performance liquid chromatography method to analyse N-methylcarbamate insecticides by a simple pose-column derivatization system and fluorescence detection[J]. Journal of Chromatography A, 1997, 778(1-2):103-110.[8] 丁涛,徐锦忠,沈崇钰,等.高效液相色谱-柱后衍生和质谱联用测定大米中氨基甲酸酯类农药残留量[J].分析试验室,2007, 26(9): 77-80.[9] SARAJI M, ESTEKI N. Analysis of carbamate pesticides in water samples using single-drop microextraction and gas chromatography-mass spectrometry[J]. Analytical and Bioanalytical Chemistry, 2008, 391(3): 1091-1100.[10] RAO T N, LOO B H, SARADA B V, et al. Electrochemical detection of carbamate pesticides at conductive diamond electrodes[J]. Analytical Chemistry, 2002, 74(7): 1578-1583.[11] CHENG X, WANG Q J, ZHANG S, et al. Determination of four kinds of carbamate pesticides by capillary zone electrophoresis with amperometric detection at a polyamide-modified carbon paste electrod[J]. Talanta, 2007, 71(3): 1083-1087.[12] SANTALAD A, ZHOU L, SHANG F J, et al. Micellar electrokinetic chromatography with amperometric detection and off-line solid-phase extraction for analysis of carbamate insecticides[J]. Journal of Chromatography A, 2010, 1217(32):5288-5297.[13] ROSSI M, ROTILIO D. Analysis of carbamate pesticides by micellar electrokinetic chromatography[J]. Journal of High Resolution Chromatography, 1997, 20(5):265-269.[14] MORENO-GONZALEZ D, GAMIZ-GRACIA L, GARCIA-CAMPANA A M, et al. Use of dispersive liquid–liquid microextraction for the determination of carbamates in juice samples by sweeping-micellar electrokinetic chromatography[J]. Analytical and Bioanalytical Chemistry, 2011, 400(5):1329-1338.[15] SUN Y, LIANG L Y, ZHAO X Y, et al. Determination of aromatic amines in water samples by capillary electrophoresis with amperometric detection[J]. Water Research, 2009, 43(1): 41-46.
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