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使用软木塞作为绿色高通量方法的平行一次性移液器萃取(Pa-DPX),用于通过HPLC-DAD定量测定环境水样中的四种农药。

Parallel-disposable pipette extraction (Pa-DPX) using cork as a green high-throughput method for the determination of four pesticides in environmental water samples with quantification by HPLC-DAD.

作者信息

Garcia Gabriela Ferreira Negro, Will Camila, Carasek Eduardo

机构信息

Chemistry Department, Federal University of Santa Catarina, Florianópolis, 88040900, Brazil.

出版信息

Anal Bioanal Chem. 2025 Mar;417(7):1359-1368. doi: 10.1007/s00216-024-05625-x. Epub 2024 Nov 2.

DOI:10.1007/s00216-024-05625-x
PMID:39488672
Abstract

This study utilized cork powder as a green alternative for extractor phase using the parallel-disposable pipette extraction (Pa-DPX) method for the determination of pesticides such as atrazine, carbofuran, diuron, and simazine from aqueous environmental samples. The separation/detection was performed by HPLC-DAD. Optimization experimental conditions was achieved through univariate and multivariate designs, resulting in the following parameters: 15 mg of cork as extractor phase, 7 extraction cycles with 7.5% (m/v) NaCl in the sample, and 10 s were fixed per extraction cycle. For the desorption step, 300 µL of acetonitrile was used as solvent with 1 desorption cycle. The limit of detection and limit of quantification values were 7.5 µg L and 25 µg L for atrazine, carbofuran, and diuron, and 15.1 µg L and 50 µg L for simazine, respectively. Linear working range varied from 25 to 400 µg L with coefficients of determination (R) ≥ 0.983. The values of intraday precision varied from 4.9 to 18.1%, and those of interday precision varied from 21.3 to 32.2%. The accuracy of the method was determined through relative recoveries and the values ranged from 63.4 to 119.9%. The water environmental samples were collected at two different locations in Florianópolis, Santa Catarina, Brazil, and showed no detectable pesticides. The method presented here stands out due to the low consumption of sample and reagents, as well as the use of a renewable and biodegradable extraction phase (cork). The method is also a high-throughput alternative, due to the use of the Pa-DPX apparatus, which allows the preparation of up to five samples simultaneously.

摘要

本研究使用软木粉作为萃取相的绿色替代品,采用平行一次性移液器萃取(Pa-DPX)方法,用于测定水环境样品中的农药,如阿特拉津、克百威、敌草隆和西玛津。分离/检测通过高效液相色谱-二极管阵列检测器(HPLC-DAD)进行。通过单变量和多变量设计实现了优化实验条件,得到以下参数:15毫克软木作为萃取相,样品中含7.5%(m/v)氯化钠进行7次萃取循环,每次萃取循环固定为10秒。对于解吸步骤,使用300微升乙腈作为溶剂进行1次解吸循环。阿特拉津、克百威和敌草隆的检测限和定量限分别为7.5微克/升和25微克/升,西玛津的检测限和定量限分别为15.1微克/升和50微克/升。线性工作范围为25至400微克/升,决定系数(R)≥0.983。日内精密度值在4.9%至18.1%之间,日间精密度值在21.3%至32.2%之间。通过相对回收率确定了该方法的准确度,其值在63.4%至119.9%之间。在巴西圣卡塔琳娜州弗洛里亚诺波利斯的两个不同地点采集了水环境样品,未检测到农药。本文提出的方法因样品和试剂消耗低以及使用可再生和可生物降解的萃取相(软木)而脱颖而出。由于使用了Pa-DPX装置,该方法也是一种高通量替代方法,可同时制备多达五个样品。

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