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超声辅助表面活性剂增强乳化微萃取-高效液相色谱法测定水样中氨基甲酸酯类农药。

Ultrasound-assisted surfactant-enhanced emulsification microextraction for the determination of carbamate pesticides in water samples by high performance liquid chromatography.

机构信息

Key Laboratory of Bioinorganic Chemistry, College of Science, Agricultural University of Hebei, Baoding, Hebei, China.

出版信息

J Chromatogr A. 2010 Mar 12;1217(11):1773-8. doi: 10.1016/j.chroma.2010.01.060. Epub 2010 Jan 25.

Abstract

A novel ultrasound-assisted surfactant-enhanced emulsification microextraction (UASEME) coupled with high performance liquid chromatography-diode array detection has been developed for the extraction and determination of six carbamate pesticides (metolcarb, carbofuran, carbaryl, pirimicarb, isoprocarb and diethofencarb) in water samples. In the UASEME technique, Tween 20 was used as emulsifier, and chlorobenzene and chloroform were used as dual extraction solvent without using any organic dispersive solvent that is normally required in the previously described common dispersive liquid-liquid microextraction method. Parameters that affect the extraction efficiency, such as the kind and volume of the extraction solvent, the type and concentration of the surfactant, ultrasound emulsification time and salt addition, were investigated and optimized for the method. Under the optimum conditions, the enrichment factors were in the range between 170 and 246. The limits of detection of the method were 0.1-0.3 ng mL(-1) and the limits of quantification were between 0.3 and 0.9 ng mL(-1), depending on the compounds. The linearity of the method was obtained in the range of 0.3-200 ng mL(-1) for metolcarb, carbaryl, pirimicarb, and diethofencarb, 0.6-200 ng mL(-1) for carbofuran, and 0.9-200 ng mL(-1) for isoprocarb, with the correlation coefficients (r) ranging from 0.9982 to 0.9998. The relative standard deviations varied from 3.2 to 4.8% (n=5). The recoveries of the method for the six carbamates from water samples at spiking levels of 1.0, 10.0, 50.0 and 100.0 ng mL(-1) were ranged from 81.0 to 97.5%. The proposed UASEME technique has demonstrated to be simple, practical and environmentally friendly for the determination of carbamates residues in river, reservoir and well water samples.

摘要

一种新型的超声辅助表面活性剂强化乳化微萃取(UASEME)与高效液相色谱-二极管阵列检测相结合,已被开发用于水样中六种氨基甲酸酯类农药(灭多威、克百威、西维因、抗蚜威、异丙威和涕灭威)的提取和测定。在 UASEME 技术中,Tween 20 被用作乳化剂,氯苯和氯仿被用作双重萃取溶剂,而无需使用通常在以前描述的常见分散液-液微萃取方法中所需的任何有机分散溶剂。研究并优化了影响萃取效率的参数,如萃取溶剂的种类和体积、表面活性剂的类型和浓度、超声乳化时间和加盐量等。在最佳条件下,富集因子在 170 到 246 之间。该方法的检出限为 0.1-0.3ng/mL,定量限为 0.3-0.9ng/mL,具体取决于化合物。该方法在 0.3-200ng/mL 范围内对灭多威、西维因、抗蚜威和涕灭威具有线性,在 0.6-200ng/mL 范围内对克百威具有线性,在 0.9-200ng/mL 范围内对异丙威具有线性,相关系数(r)范围为 0.9982 至 0.9998。该方法在 1.0、10.0、50.0 和 100.0ng/mL 加标水平下测定水样中六种氨基甲酸酯的相对标准偏差为 3.2%-4.8%(n=5)。该方法对河水、水库水和井水样品中六种氨基甲酸酯的回收率在 81.0%-97.5%之间。该提议的 UASEME 技术已被证明在测定河水中的氨基甲酸酯残留方面具有简单、实用和环保的特点。

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