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采用多壁碳纳米管(MWCNTs)和毛细管电泳法快速测定水样中氯磺隆和甲磺隆的方法。

A simple and fast method for chlorsulfuron and metsulfuron methyl determination in water samples using multiwalled carbon nanotubes (MWCNTs) and capillary electrophoresis.

机构信息

FIA Laboratory, Analytical Chemistry Section, INQUISUR (UNS-CONICET), Av. Alem 1253, B8000CPB Bahía Blanca, Buenos Aires, Argentina.

出版信息

Talanta. 2010 Nov 15;83(1):126-9. doi: 10.1016/j.talanta.2010.08.049. Epub 2010 Sep 24.

Abstract

A new method to determine metsulfuron methyl (MSM) and chlorsulfuron (CS) in different water samples was developed. It consists in a solid phase extraction (SPE) procedure using multiwalled carbon nanotubes (MWCNTs) as sorbent material in combination with capillary zone electrophoretic determination. To carry out the pre-concentration step, a simple flow injection system was developed and optimized. Thus, 250 μL of aqueous solution containing methanol 50% (v/v) and acetonitrile 2% (v/v) as eluent, 10 mL of sample and a flow rate of 1.15 mL min(-1) were selected. The CE variables also were optimized. A rapid determination and good resolution of two herbicides were obtained within 9 min using a simple electrophoretic buffer (50 mmol L(-1) sodium tetraborate with 3% of methanol, pH=9.0). Under the optimum conditions, the calibration curves were linear between 0.5 and 6 μg L(-1) for MSM and CS with R(2)=0.995 and 0.997, respectively. The repeatability of the proposed method, expressed as relative standard deviation (RSD), varied between 4.1% and 5.4% (n=10) and the detection limits for MSM and CS were 0.40 and 0.36 μg L(-1), respectively. Good results were achieved when the proposed method was applied to spiked real water samples. The recoveries percentages of the two analytes were over the range 86-108%.

摘要

一种新的方法来测定不同水样中的甲磺隆(MSM)和氯磺隆(CS)。它由固相萃取(SPE)程序,使用多壁碳纳米管(MWCNTs)作为吸附材料,结合毛细管区带电泳测定。为了进行预浓缩步骤,开发并优化了一种简单的流动注射系统。因此,选择了含有甲醇 50%(v/v)和乙腈 2%(v/v)的洗脱液 250 μL、10 mL 样品和 1.15 mL min(-1)的流速。还优化了 CE 变量。使用简单的电泳缓冲液(50 mmol L(-1)四硼酸钠,含 3%甲醇,pH=9.0),在 9 min 内可快速测定和良好分离两种除草剂。在最佳条件下,MSM 和 CS 的校准曲线在 0.5 和 6 μg L(-1)之间呈线性,相关系数分别为 0.995 和 0.997。所提出方法的重复性,用相对标准偏差(RSD)表示,在 4.1%至 5.4%(n=10)之间变化,MSM 和 CS 的检测限分别为 0.40 和 0.36 μg L(-1)。当将该方法应用于加标实际水样时,可获得良好的结果。两种分析物的回收率百分比均在 86-108%范围内。

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