Multivariate optimization of dispersive liquid-liquid microextraction solvent-based for the determination of organochlorine pesticides in water by gas chromatography coupled to mass spectrometry

IF 3.4 4区化学 Q2 CHEMISTRY, MULTIDISCIPLINARY

Journal of the Indian Chemical Society Pub Date : 2025-09-30 DOI:10.1016/j.jics.2025.102154

Flavianny Brencis da Silva Mikalouski , Ana Claudia Ueda , Edmilson Antônio Canesin , Graciana Freitas Palioto , Jéssica Guerreiro Martins , Tayssa Nogueira da Silva , Udson Mikalouski , Sharise Beatriz Roberto Berton , Jomar Berton Junior , Rúbia Michele Suzuki

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Abstract

In this work, a dispersive liquid-liquid microextraction (DLLME) method was optimized for the determination of organochlorine pesticides in water samples, including surface water. Chloroform was used as the extraction solvent, and acetone was used as the dispersive solvent. Initially, solvent selection was performed univariately. Subsequently, key parameters, such as the type of extraction solvent, temperature, and volumes of extraction and dispersive solvents, were optimized using a full factorial design. The optimized conditions included an extraction temperature of 5 and 20 °C, and an extraction solvent volume of 25 μL and 50 μL. Coupled with gas chromatography-mass spectrometry (GC-MS), the method demonstrates detection limits ranging from 1.16 to 9.91 ng L⁻¹ and quantification limits from 3.51 to 30.0 ng L⁻¹. The developed method proved effective for detecting organochlorine pesticides (α-BHC, β-BHC, γ-BHC, Heptachlor, Heptachlor epoxide, Aldrin, Dieldrin, 4,4′-DDE, 4,4′-DDD, and 4,4′-DDT), offering a simple and efficient alternative for environmental monitoring and analysis.

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基于分散液液微萃取溶剂的气相色谱-质谱联用测定水中有机氯农药的多元优化

本研究优化了分散液液微萃取法（DLLME）测定地表水等水样中有机氯农药的方法。以氯仿为萃取溶剂，丙酮为分散溶剂。最初，溶剂选择是单因素进行的。随后，利用全因子设计对提取溶剂类型、温度、提取溶剂和分散溶剂的体积等关键参数进行了优化。优化条件为：提取温度为5℃、20℃，提取溶剂体积为25 μL、50 μL。结合气相色谱-质谱（GC-MS），该方法的检出限为1.16 ~ 9.91 ng L−1，定量限为3.51 ~ 30.0 ng L−1。该方法对有机氯农药（α-六六六、β-六六六、γ-六六六、七氯、环氧七氯、Aldrin、Dieldrin、4,4′-DDE、4,4′-DDD、4,4′-DDT）的检测具有较好的检测效果，为环境监测和分析提供了一种简便、高效的方法。

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来源期刊

Journal of the Indian Chemical Society 化学-化学综合

CiteScore

3.50

自引率

7.70%

发文量

492

审稿时长

3-8 weeks

期刊介绍： The Journal of the Indian Chemical Society publishes original, fundamental, theorical, experimental research work of highest quality in all areas of chemistry, biochemistry, medicinal chemistry, electrochemistry, agrochemistry, chemical engineering and technology, food chemistry, environmental chemistry, etc.