Solid-phase microextraction and gas chromatography-mass spectrometry for quantitative determination of chlordecone in water, plant and soil samples

Abstract

-Introduction. Chlordecone (CLD), an organochlorine formerly used to control the banana black weevil, is strongly adsorbed on soils, particularly on andosols. A simplified analytical procedure for the quantitative determination of chlordecone residues in water and micro-samples of soil and plants was compared with a standard method. Materials and methods. The procedure combines a simplified sampling protocol and a 10-min solid phase microextraction (SPME), followed by gas chromatographic separation (GC) and mass spectrometric (MS and MS/MS) identification. Quantitation of CLD used a standard addition method with zero extrapolation. First, seventy samples were analysed using the proposed method and the standard method based on hot solvent extraction. Second, fifteen soil samples were analysed with two SPME methods followed by GC-MS but using CLD labelled with C 13 as an internal standard or the proposed method. Results and discussion. The detection (LOD) and quantitation (LOQ) limits of our SPME extraction procedure were determined for GC-MS and GC-MS/MS with water, plant (pineapple roots) and soil samples: in water for MS/MS, LOD MS/MS-water = 0.5 ng⋅L -1 , LOQ MS/MS-water = 2.0 ng⋅L -1 ; in andosol for MS/MS, LOD MS/MS-soil = 15.0 ng⋅kg -1 dw, LOQ MS/MS-soil = 80.0 ng⋅kg -1 dw. Data from the seventy contaminated soils obtained with the proposed method and the standard method showed a correlation coefficient of r = 0.86. Data obtained by the two SPME/GC-MS quantitation procedures showed a correlation of r = 0.8073. Conclusion. The method proposes a simplified sample preparation and extraction of CLD in water, plant and soil samples, with no solvent manipulation and which is not time-consuming. The LOD and LOQ were similar to those obtained with other currently used methods. The method is reliable and accurate and may be considered as a good tool for research purposes. Résumé -Introduction. La chlordécone (CLD), organochloré autrefois utilisé contre le charançon noir du bananier, est fortement adsorbée sur les sols, comme les andosols. Une procédure simplifiée pour la détermination quantitative des résidus de CLD dans l'eau et des micro-échantillons de sol et de plantes a été comparée à une méthode standard. Matériels et méthodes. La procédure associe un échantillonnage simplifié, une micro-extraction en phase solide (SPME) de 10 min, une séparation par chromatographie en phase gazeuse (GC) et une identification par spectrométrie de masse (MS et MS/MS). La quantification est basée sur une méthode d'ajouts dosés. Soixante-dix échantillons ont été analysés en utilisant la méthode proposée et la méthode standard (extraction par solvant à chaud). Quinze échantillons de sol ont été analysés par deux méthodes SPME GC-MS, mais avec comme étalon interne la CLD C 13 ou la méthode proposée. Résultats et discussion. Les limites de détection (LOD) et de quantification (LOQ) ont été déterminées pour la GC-MS et la GC-MS/MS dans l'eau, dans des plantes (racines d'ananas) et dans les sols : dans l'eau pour la MS/MS, LO...

Fluorescence Detection of the Persistent Organic Pollutant Chlordecone in Water at Environmental Concentrations

“…Notably, it still contaminates the hydric system, soils, the food chain and consequently humans [12] . Furthermore, even if several analytical techniques have been developed over the years to quantify and monitor chlordecone (Table S1), they suffer from two major limitations: firstly, they require rather expensive devices and equipment (e. g. GC‐MS/MS and LC–MS/MS); secondly, moderate to high uncertainties remain due to the strong fixation of chlordecone on organic matter [13–15] . Thus, a convenient, fast, cheap and robust method to detect chlordecone in water and which can be directly performed on the polluted sites has still to be developed.…”

Determination of 1-methyl-1H-1,2,4-triazole in soils contaminated by rocket fuel using solid-phase microextraction, isotope dilution and gas chromatography–mass spectrometry

“…Addition of excess water [22][23][24][25][26][27]; preliminary extraction by organic solvent followed by its evaporation and addition of excess water [28,29]; exhaustive extraction by cold SPME fiber [30,31]; standard addition [23]; and internal standard [20,22,32].…”

Physico-chemical and agronomic results of soil remediation by In Situ Chemical Reduction applied to a chlordecone-contaminated nitisol at plot scale in a French Caribbean banana plantation

“…The analytical procedure combined solid-phase micro-extraction (SPME) for 10 minutes, separation by gas chromatography (GC) and identification by mass spectrometry (MS and MS/MS). Quantification was based on a standard addition method (Soler et al, 2014).…”