{"title":"Development of thin film microextraction method for the multi-residue analysis of selected pesticides","authors":"Kübra Kahremanoğlu , Yeliz Akpınar , Ezel Boyaci","doi":"10.1016/j.sampre.2023.100061","DOIUrl":null,"url":null,"abstract":"<div><p>Pesticides are a class of compounds that are used to protect agricultural products. However, the uncontrolled use of these chemicals increases the risks associated with their overdosing and rises a significant concern about their effect on human health and the ecosystem. Albeit many concerns about their effects, the use of pesticides is inevitable due to the incline in population growth and the presence of limited food resources. As a result, regulatory control of the use of chemicals is critical and the development of methods that provide a reliable determination of pesticide residues in fruits and vegetables is of great importance.</p><p>In the present study, a new method based on thin film microextraction was developed for the extraction of pesticides from fruit matrices prior to their gas chromatography-mass spectrometric (GC–MS) determination. As a first step, the thin film extractive devices were prepared by immobilization of hydrophilic-lipophilic balanced (HLB) particles on the surface of carbon mesh. The samplers were optimized in terms of extraction and desorption conditions first in PBS and then in apple juice. The final method was also validated in apple juice samples. Analytical figures of merits of the final method showed acceptable precision for intra- and inter-day reproducibility with ≤20% relative standard deviation (RSD%) and accuracy of ≤15% relative error (RE%), except for trifluralin at 300.0 ng mL<sup>−1</sup> level. The limits of quantitation (LOQ) for the selected pesticides were found between 1.0 and 5.0 ng mL<sup>−1</sup> . The samplers developed in this study were also successfully tested in preliminary investigations for the extraction of the pesticides from the surface of fruits and vegetables using agarose gel as a model matrix with the primary aim of showing the step towards the sampling directly on the field.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"6 ","pages":"Article 100061"},"PeriodicalIF":5.2000,"publicationDate":"2023-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"1","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Advances in Sample Preparation","FirstCategoryId":"1085","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S2772582023000116","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
引用次数: 1
Abstract
Pesticides are a class of compounds that are used to protect agricultural products. However, the uncontrolled use of these chemicals increases the risks associated with their overdosing and rises a significant concern about their effect on human health and the ecosystem. Albeit many concerns about their effects, the use of pesticides is inevitable due to the incline in population growth and the presence of limited food resources. As a result, regulatory control of the use of chemicals is critical and the development of methods that provide a reliable determination of pesticide residues in fruits and vegetables is of great importance.
In the present study, a new method based on thin film microextraction was developed for the extraction of pesticides from fruit matrices prior to their gas chromatography-mass spectrometric (GC–MS) determination. As a first step, the thin film extractive devices were prepared by immobilization of hydrophilic-lipophilic balanced (HLB) particles on the surface of carbon mesh. The samplers were optimized in terms of extraction and desorption conditions first in PBS and then in apple juice. The final method was also validated in apple juice samples. Analytical figures of merits of the final method showed acceptable precision for intra- and inter-day reproducibility with ≤20% relative standard deviation (RSD%) and accuracy of ≤15% relative error (RE%), except for trifluralin at 300.0 ng mL−1 level. The limits of quantitation (LOQ) for the selected pesticides were found between 1.0 and 5.0 ng mL−1 . The samplers developed in this study were also successfully tested in preliminary investigations for the extraction of the pesticides from the surface of fruits and vegetables using agarose gel as a model matrix with the primary aim of showing the step towards the sampling directly on the field.
农药是一类用于保护农产品的化合物。然而,这些化学品的不受控制的使用增加了与过量使用相关的风险,并引发了人们对其对人类健康和生态系统影响的严重担忧。尽管人们对杀虫剂的影响有很多担忧,但由于人口增长的趋势和有限的粮食资源,杀虫剂的使用是不可避免的。因此,对化学品使用的监管至关重要,开发可靠测定水果和蔬菜中农药残留的方法至关重要。在本研究中,开发了一种基于薄膜微萃取的新方法,用于在气相色谱-质谱(GC–MS)测定之前从水果基质中提取农药。作为第一步,通过将亲水-亲脂性平衡(HLB)颗粒固定在碳网表面来制备薄膜萃取装置。首先在PBS中,然后在苹果汁中对采样器的提取和解吸条件进行了优化。最后的方法也在苹果汁样品中得到了验证。最终方法优点的分析图显示,日内和日间再现性的精密度可接受,相对标准偏差(RSD%)≤20%,相对误差(RE%)≤15%,但浓度为300.0 ng mL−1的氟乐灵除外。所选农药的定量限(LOQ)在1.0至5.0 ng/mL−1之间。本研究中开发的采样器也在使用琼脂糖凝胶作为模型基质从水果和蔬菜表面提取农药的初步研究中成功测试,主要目的是显示直接在现场采样的步骤。