HPLC Determination of Carbofuran in Water with Pre-enrichment by SPE
摘 要
取200 mL水样,流经C18固相萃取(SPE)小柱富集呋喃丹。用5.0 mL四氢呋喃从SPE柱上洗脱呋喃丹,收集洗脱液,在35 ℃吹氩蒸干。用1.0 mL甲醇溶解残渣,所得溶液供高效液相色谱分析。用Eclipse XDB C18色谱柱及由甲醇-水(1+1)混合溶液作流动相进行分离,并以285 nm作激发波长,320 nm作发射波长对呋喃丹作荧光检测。测得呋喃丹的质量浓度在5.0×10-4~5.0 mg·L-1范围内与相应的峰面积值呈线性关系,检出限(3S/N)为0.02 μg·L-1。以水样为基体加入3个浓度水平(1.0,50.0,200.0 μg·L-1)标准溶液对方法作回收及精密度试验,测得回收率在94.0%~99.6%之间,相对标准偏差(n=7)在1.2%~4.2%之间。
Abstract
Two hundred mL of water sample were taken and passed through C18 SPE column to enrich trace amount of carbofuran on the column. Five mL of tetrahydrofuran were used to elute carbofuran from the column, and the eluate was evaporated to dryness by Ar-blowing at 35 ℃. The residue was taken up with 1.0 mL of methanol which was used for HPLC analysis. The Eclipse XDB C18 chromatographic column and the mobile phase of mixture of methanol and water (1+1) were used for separation. Fluorescence detection at λex of 285 nm and λem of 320 nm was adopted in the determination. Linear relationship between values of peak area and mass concentration of carbofuran was obtained in the range of 5×10-4-5.0 mg·L-1, with detection limit (3S/N) of 0.02 μg·L-1. Recovery and precision were tested on water samples by standard addition method at 3 concentration levels of 1.0, 50.0, 200.0 μg·L-1, giving results of recovery in the range of 94.0%-99.6% and RSD′s (n=7) in the range of 1.2%-4.2%.
中图分类号 O652.63
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基金项目 中央级公益性科研院所基本科研业务费专项资金项目(K-JBYWF-2009-T203);2010年中央级公益性科研院所基本科研业务费专项资金项目(K-JBYWF-2010-G17)
收稿日期 2010/1/27
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备注王晓楠(1985-),女,辽宁人,助理工程师,硕士,主要从事色谱研究。
引用该论文: WANG Xiao-nan,YAN Wei,LIU Yu. HPLC Determination of Carbofuran in Water with Pre-enrichment by SPE[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(4): 430~432
王晓楠,烟卫,刘昱. 固相萃取-高效液相色谱法测定水中呋喃丹[J]. 理化检验-化学分册, 2011, 47(4): 430~432
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参考文献
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【2】CHEN Jian-bo, ZHAO Wei-jun, LIU Wei, et al. Cloud point extraction coupled with derivative of carbofuran as a preconcentration step prior to HPLC[J]. Food Chemistry, 2009,115(3):1038-1041.
【3】BATTU R S, KALRA R L, DHILLON R S. Estimation of residues of carbofuran and its metabolites in sugarcane and soil by derivatization with 1-fluoro-2,4-dinitrobenzene and gas chromatography with nitrogen-phosphorus detection[J]. Journal of Aoac International, 2000,83(3):569-578.
【4】张鑫,丁清波.气相色谱法测定水中呋喃丹[J].环境监测管理与技术, 2007,19(2):36-38.
【5】PETROPOULOU S S E, GIKAS E, TSARBOPOULOS A, et al. Gas chromatographic-tandem mass spectrometric method for the quantitation of carbofuran, carbaryl and their main metabolites in applicators′ urine[J]. Journal of Chromatography A, 2006,1108(1):99-110.
【6】杨丽莉,胡恩宇,母应锋,等.水中呋喃丹气相色谱-质谱的测定方法研究[J].中国环境监测, 2007,23(2):17-19.
【7】郑和辉,张静,李洁,等.超高效液相色谱串联质谱法直接进样测定水中的草甘膦和呋喃丹[J].分析试验室, 2008,27:68-70.
【8】CABALLO-LPEZ A, LUQUE de CASTRO M D. Continuous ultrasound-assisted extraction coupled to on line filtration-solid-phase extraction-column liquid chromatographypost column derivatisation-fluorescence detection for the determination of N-methylcarbamates in soil and food[J]. Journal of Chromatography A, 2003,998(1/2):51-59.
【9】刘长武,刘潇威,翟广书,等.固相萃取2高效液相色谱法测定蔬菜、水果中的氨基甲酸酯杀虫剂及其代谢物残留[J].色谱, 2003,21(3):255-257.
【10】巢猛,陈明,刘建明.水中呋喃丹的固相萃取-高效液相色谱测定法[J].环境与健康杂志, 2008,25(2):153-154.
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