Green Analytical Method Using Single-Drop Microextraction Followed by Gas Chromatography for Nitro Compound Detection in Environmental Water and Forensic Rinse Water

The extensive use of nitro compounds in agriculture, industry, armaments, and pharmaceuticals, along with their toxic effects on living organisms, necessitates efficient and environmentally sustainable analytical methods. Traditional extraction techniques often involve practices that are not eco-fri...

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Main Authors: Tamara Pócsová, Senad Okanovič, Svetlana Hrouzková
Format: Article
Language:English
Published: MDPI AG 2025-04-01
Series:Molecules
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Online Access:https://www.mdpi.com/1420-3049/30/9/1894
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author Tamara Pócsová
Senad Okanovič
Svetlana Hrouzková
author_facet Tamara Pócsová
Senad Okanovič
Svetlana Hrouzková
author_sort Tamara Pócsová
collection DOAJ
description The extensive use of nitro compounds in agriculture, industry, armaments, and pharmaceuticals, along with their toxic effects on living organisms, necessitates efficient and environmentally sustainable analytical methods. Traditional extraction techniques often involve practices that are not eco-friendly, such as the use of large volumes of solvents, toxic chemicals, and the generation of significant waste; therefore, the single-drop microextraction technique was involved in overcoming these limitations. This study shows an environmentally friendly method for nitro compound analysis focusing on NB (Nitrobenzene), 2-NT (2-Nitrotoluene), 3-NT (3-Nitrotoluene), 4-NT (4-Nitrotoluene), 1,3-DNB (1,3-Dinitrobenzene), 1,2-DNB (1,2-Dinitrobenzene), 2,4-DNT (2,4-Dinitrotoluene), and TNT (Trinitrotoluene). To separate and to detect selected nitro compounds, gas chromatography with an electron capture detector was utilized, which is highly selective for analytes containing nitro groups. To determine optimal experimental conditions, extraction parameters were studied, including the impact of salt addition, temperature, and pH on extraction efficiency. Key performance parameters, such as limit of detection (LOD), limit of quantification (LOQ), repeatability, extraction recoveries, calibration range, and matrix effects, were assessed. The LOD values ranged from 0.01 to 0.09 μg/L in deionized water, 0.01 to 0.06 μg/L in tap water, 0.01 to 0.03 μg/L in seawater, and 0.03 to 0.11 μg/L in model forensic rinse water. The optimized method was successfully applied to the determination of nitro compounds in real environmental water samples and forensic rinse water samples. The environmental sustainability and greenness of the proposed method was evaluated with the AGREE, AGREEprep, and AESA techniques.
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spelling doaj-art-a07224e3da7b404a84bb3bae19ea1c1e2025-08-20T02:59:14ZengMDPI AGMolecules1420-30492025-04-01309189410.3390/molecules30091894Green Analytical Method Using Single-Drop Microextraction Followed by Gas Chromatography for Nitro Compound Detection in Environmental Water and Forensic Rinse WaterTamara Pócsová0Senad Okanovič1Svetlana Hrouzková2Faculty of Chemical and Food Technology, Institute of Analytical Chemistry, Slovak University of Technology in Bratislava, Radlinského 9, 812 37 Bratislava, SlovakiaFaculty of Chemical and Food Technology, Institute of Analytical Chemistry, Slovak University of Technology in Bratislava, Radlinského 9, 812 37 Bratislava, SlovakiaFaculty of Chemical and Food Technology, Institute of Analytical Chemistry, Slovak University of Technology in Bratislava, Radlinského 9, 812 37 Bratislava, SlovakiaThe extensive use of nitro compounds in agriculture, industry, armaments, and pharmaceuticals, along with their toxic effects on living organisms, necessitates efficient and environmentally sustainable analytical methods. Traditional extraction techniques often involve practices that are not eco-friendly, such as the use of large volumes of solvents, toxic chemicals, and the generation of significant waste; therefore, the single-drop microextraction technique was involved in overcoming these limitations. This study shows an environmentally friendly method for nitro compound analysis focusing on NB (Nitrobenzene), 2-NT (2-Nitrotoluene), 3-NT (3-Nitrotoluene), 4-NT (4-Nitrotoluene), 1,3-DNB (1,3-Dinitrobenzene), 1,2-DNB (1,2-Dinitrobenzene), 2,4-DNT (2,4-Dinitrotoluene), and TNT (Trinitrotoluene). To separate and to detect selected nitro compounds, gas chromatography with an electron capture detector was utilized, which is highly selective for analytes containing nitro groups. To determine optimal experimental conditions, extraction parameters were studied, including the impact of salt addition, temperature, and pH on extraction efficiency. Key performance parameters, such as limit of detection (LOD), limit of quantification (LOQ), repeatability, extraction recoveries, calibration range, and matrix effects, were assessed. The LOD values ranged from 0.01 to 0.09 μg/L in deionized water, 0.01 to 0.06 μg/L in tap water, 0.01 to 0.03 μg/L in seawater, and 0.03 to 0.11 μg/L in model forensic rinse water. The optimized method was successfully applied to the determination of nitro compounds in real environmental water samples and forensic rinse water samples. The environmental sustainability and greenness of the proposed method was evaluated with the AGREE, AGREEprep, and AESA techniques.https://www.mdpi.com/1420-3049/30/9/1894nitro compoundsforensic samplesenvironmental watersingle-drop microextractiongas chromatography
spellingShingle Tamara Pócsová
Senad Okanovič
Svetlana Hrouzková
Green Analytical Method Using Single-Drop Microextraction Followed by Gas Chromatography for Nitro Compound Detection in Environmental Water and Forensic Rinse Water
Molecules
nitro compounds
forensic samples
environmental water
single-drop microextraction
gas chromatography
title Green Analytical Method Using Single-Drop Microextraction Followed by Gas Chromatography for Nitro Compound Detection in Environmental Water and Forensic Rinse Water
title_full Green Analytical Method Using Single-Drop Microextraction Followed by Gas Chromatography for Nitro Compound Detection in Environmental Water and Forensic Rinse Water
title_fullStr Green Analytical Method Using Single-Drop Microextraction Followed by Gas Chromatography for Nitro Compound Detection in Environmental Water and Forensic Rinse Water
title_full_unstemmed Green Analytical Method Using Single-Drop Microextraction Followed by Gas Chromatography for Nitro Compound Detection in Environmental Water and Forensic Rinse Water
title_short Green Analytical Method Using Single-Drop Microextraction Followed by Gas Chromatography for Nitro Compound Detection in Environmental Water and Forensic Rinse Water
title_sort green analytical method using single drop microextraction followed by gas chromatography for nitro compound detection in environmental water and forensic rinse water
topic nitro compounds
forensic samples
environmental water
single-drop microextraction
gas chromatography
url https://www.mdpi.com/1420-3049/30/9/1894
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AT senadokanovic greenanalyticalmethodusingsingledropmicroextractionfollowedbygaschromatographyfornitrocompounddetectioninenvironmentalwaterandforensicrinsewater
AT svetlanahrouzkova greenanalyticalmethodusingsingledropmicroextractionfollowedbygaschromatographyfornitrocompounddetectioninenvironmentalwaterandforensicrinsewater