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非离子表面活性剂胶束电动色谱-激光诱导荧光检测法同时测定含磷氨基酸类除草剂

Simultaneous determination of phosphorus-containing amino acid-herbicides by nonionic surfactant micellar electrokinetic chromatography with laser-induced fluorescence detection.

作者信息

Molina M, Silva M

机构信息

Department of Analytical Chemistry and Ecology, University of Córdoba, Spain.

出版信息

Electrophoresis. 2001 Apr;22(6):1175-81. doi: 10.1002/1522-2683()22:6<1175::AID-ELPS1175>3.0.CO;2-8.

Abstract

The potential of micellar electrokinetic chromatography (MEKC) with laser-induced fluorescence (LIF) detection for the separation and determination of phosphorus-containing amino acid-herbicides (glufosinate and glyphosate), and aminomethylphosphonic acid (the major metabolite of glyphosate), involving derivatization with fluorescein isothiocyanate (FITC) isomer I, was investigated. Different variables that affect derivatization (pH, FITC concentration, time and temperature) and separation (pH and concentration of the buffer, kind and concentration of surfactants and applied voltage) were studied. The analysis was conducted within about 8 min and the use of the nonionic surfactant Triton X-100 improved the selectivity, thus indirectly enhancing sensitivity by shifting of the interfering peaks of the FITC excess. Dynamic ranges of 2.0-3,000 microg/L, limits of detection at microgram or submicrogram-per-liter level, and relative standard deviations from 4.7 to 6.4% were obtained. The ensuing method--nonionic surfactant MEKC-- is a useful choice for the determination of these herbicides as it provides limits of detection similar or lower than those reported by existing chromatographic alternatives without the use of an additional preconcentration technique such as solid-phase extraction. The separation of a mixture of nine FITC-derivatized amino acids, selected as target compounds, was also carried out to assess the discrimination power of the nonionic surfactant MEKC method for the analysis of closely related anionic analytes.

摘要

研究了采用激光诱导荧光(LIF)检测的胶束电动色谱(MEKC)用于分离和测定含磷氨基酸除草剂(草铵膦和草甘膦)以及氨甲基膦酸(草甘膦的主要代谢物)的潜力,其中涉及用异硫氰酸荧光素(FITC)异构体I进行衍生化。研究了影响衍生化的不同变量(pH值、FITC浓度、时间和温度)以及分离的变量(缓冲液的pH值和浓度、表面活性剂的种类和浓度以及施加电压)。分析在约8分钟内完成,使用非离子表面活性剂Triton X-100提高了选择性,从而通过FITC过量干扰峰的偏移间接提高了灵敏度。获得了2.0 - 3000 μg/L的动态范围、微克或亚微克每升水平的检测限以及4.7%至6.4%的相对标准偏差。随后的方法——非离子表面活性剂MEKC——是测定这些除草剂的一种有用选择,因为它提供的检测限与现有色谱方法报道的相似或更低,且无需使用额外的预浓缩技术如固相萃取。还对作为目标化合物选择的九种FITC衍生化氨基酸的混合物进行了分离,以评估非离子表面活性剂MEKC方法对密切相关阴离子分析物的分辨能力。

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