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采用定制装置开发绿色液相微萃取程序,综合测定不同类型葡萄酒样品中的传统和新型农药。

Development of a green liquid-phase microextraction procedure using a customized device for the comprehensive determination of legacy and current pesticides in distinct types of wine samples.

机构信息

Centro Universitário SENAI-CIMATEC, Av. Orlando Gomes, 1845 - Piatã, 41650-010, Salvador, BA, Brazil; Instituto Nacional de Ciência e Tecnologia Em Energia e Ambiente - INCT E&A, Universidade Federal da Bahia, 40170-115, Salvador, BA, Brazil; Centro Interdisciplinar de Energia e Ambiente - CIEnAm, Universidade Federal da Bahia, 40170-115, Salvador, BA, Brazil.

Centro Universitário SENAI-CIMATEC, Av. Orlando Gomes, 1845 - Piatã, 41650-010, Salvador, BA, Brazil; Instituto Nacional de Ciência e Tecnologia Em Energia e Ambiente - INCT E&A, Universidade Federal da Bahia, 40170-115, Salvador, BA, Brazil.

出版信息

Talanta. 2024 Jan 1;266(Pt 1):124914. doi: 10.1016/j.talanta.2023.124914. Epub 2023 Jul 11.

Abstract

In this work, we reported the development of a novel, simple, and green liquid-phase microextraction (LPME) procedure based on the use of a customized device for the determination of 47 multiclass pesticides in red, white, and rosè wine samples by GC-MS. The main parameters that affect the LPME were optimized using multivariate statistical techniques such as centroid-simplex mixture design and Doehlert design. The optimal conditions were: 70 μL of toluene as extractor solvent; concentration of NaCl (2.7%, m v); pH 4; and an extraction time of 30 min, under vortex-assisted agitation (at 500 rpm). After validation, it was possible to obtain LOQ values as low as 7.63 ng L and extraction recoveries ranging from 81.7% to 119% for most of the target pesticides. The application of exploratory analysis, specifically Principal Component Analysis (PCA) and Hierarchical Cluster Analysis (HCA), provided evidence indicating contamination in the different types of wine samples, primarily by systemic fungicides.

摘要

在这项工作中,我们报告了一种新的、简单的、绿色的液相微萃取(LPME)方法的发展,该方法基于使用定制设备,通过 GC-MS 测定红、白和玫瑰葡萄酒样品中的 47 种多类农药。使用多元统计技术(如质心单纯形混合设计和 Doehlert 设计)优化了影响 LPME 的主要参数。最佳条件为:70μL 甲苯作为萃取溶剂;NaCl 浓度(2.7%,m/v);pH 值 4;涡旋辅助搅拌下(500rpm)提取 30min。经过验证,可以获得低至 7.63ng/L 的 LOQ 值和大多数目标农药的萃取回收率在 81.7%至 119%之间。探索性分析,特别是主成分分析(PCA)和层次聚类分析(HCA)的应用,提供了证据表明不同类型的葡萄酒样品受到了污染,主要是由系统性杀菌剂引起的。

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