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Simultaneous determination of traces of pyrethroids, organochlorines and other main plant protection agents in agricultural soils by headspace solid-phase microextraction-gas chromatography.
J Chromatogr A. 2008 Apr 25; 1188(2):154-63.JC

Abstract

A solvent-free and simple method based on headspace solid-phase microextraction (HS-SPME) was developed in order to determine simultaneously 36 common pesticides and breakdown products (mostly pyrethroids and organochlorine compounds) in soil. The analysis was carried out by gas chromatography with micro-electron-capture detection (GC-microECD). As far as we know, this is the first study about the SPME of pyrethroid insecticides from soil. Factors such as extraction temperature, matrix modification by addition of water, salt addition (% NaCl) and fiber coating were considered in the optimization of the HS-SPME. To this end, a 3 x 2(3-1) fractional factorial design was performed. The results showed that temperature and fiber coating were the most significant variables affecting extraction efficiency. A suitable sensitivity for all investigated compounds was achieved at 100 degrees C by extracting soil samples wetted with 0.5 mL of ultrapure water (0% NaCl) employing a polyacrylate (PA) coating fiber. Using the recommended extraction conditions with GC-microECD, a linear calibration could be achieved over a range of two orders of magnitude for both groups of analytes. Limits of detection (LODS) at the sub-ng g(-1) level were attained and relative standard deviations (RSDs) were found to be lower than 14% for both groups of pesticides. Matrix effects were investigated by the analysis of different soil samples fortified with the target compounds. The method accuracy was assessed and good recovery values (>70%, in most cases) were obtained. The method was also validated with a certified reference material (RTC-CRM818-050), which was quantified using a standard addition protocol. Finally, the proposed HS-SPME-GC-microECD methodology was further applied to the screening of environmental soil samples for the presence of the target pesticides.

Authors+Show Affiliations

Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Campus Sur, Universidad de Santiago de Compostela, E-15706 Santiago de Compostela, Spain.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

18346746

Citation

Fernandez-Alvarez, Maria, et al. "Simultaneous Determination of Traces of Pyrethroids, Organochlorines and Other Main Plant Protection Agents in Agricultural Soils By Headspace Solid-phase Microextraction-gas Chromatography." Journal of Chromatography. A, vol. 1188, no. 2, 2008, pp. 154-63.
Fernandez-Alvarez M, Llompart M, Lamas JP, et al. Simultaneous determination of traces of pyrethroids, organochlorines and other main plant protection agents in agricultural soils by headspace solid-phase microextraction-gas chromatography. J Chromatogr A. 2008;1188(2):154-63.
Fernandez-Alvarez, M., Llompart, M., Lamas, J. P., Lores, M., Garcia-Jares, C., Cela, R., & Dagnac, T. (2008). Simultaneous determination of traces of pyrethroids, organochlorines and other main plant protection agents in agricultural soils by headspace solid-phase microextraction-gas chromatography. Journal of Chromatography. A, 1188(2), 154-63. https://doi.org/10.1016/j.chroma.2008.02.080
Fernandez-Alvarez M, et al. Simultaneous Determination of Traces of Pyrethroids, Organochlorines and Other Main Plant Protection Agents in Agricultural Soils By Headspace Solid-phase Microextraction-gas Chromatography. J Chromatogr A. 2008 Apr 25;1188(2):154-63. PubMed PMID: 18346746.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous determination of traces of pyrethroids, organochlorines and other main plant protection agents in agricultural soils by headspace solid-phase microextraction-gas chromatography. AU - Fernandez-Alvarez,Maria, AU - Llompart,Maria, AU - Lamas,J Pablo, AU - Lores,Marta, AU - Garcia-Jares,Carmen, AU - Cela,Rafael, AU - Dagnac,Thierry, Y1 - 2008/03/02/ PY - 2007/12/14/received PY - 2008/02/22/revised PY - 2008/02/22/accepted PY - 2008/3/19/pubmed PY - 2008/7/9/medline PY - 2008/3/19/entrez SP - 154 EP - 63 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1188 IS - 2 N2 - A solvent-free and simple method based on headspace solid-phase microextraction (HS-SPME) was developed in order to determine simultaneously 36 common pesticides and breakdown products (mostly pyrethroids and organochlorine compounds) in soil. The analysis was carried out by gas chromatography with micro-electron-capture detection (GC-microECD). As far as we know, this is the first study about the SPME of pyrethroid insecticides from soil. Factors such as extraction temperature, matrix modification by addition of water, salt addition (% NaCl) and fiber coating were considered in the optimization of the HS-SPME. To this end, a 3 x 2(3-1) fractional factorial design was performed. The results showed that temperature and fiber coating were the most significant variables affecting extraction efficiency. A suitable sensitivity for all investigated compounds was achieved at 100 degrees C by extracting soil samples wetted with 0.5 mL of ultrapure water (0% NaCl) employing a polyacrylate (PA) coating fiber. Using the recommended extraction conditions with GC-microECD, a linear calibration could be achieved over a range of two orders of magnitude for both groups of analytes. Limits of detection (LODS) at the sub-ng g(-1) level were attained and relative standard deviations (RSDs) were found to be lower than 14% for both groups of pesticides. Matrix effects were investigated by the analysis of different soil samples fortified with the target compounds. The method accuracy was assessed and good recovery values (>70%, in most cases) were obtained. The method was also validated with a certified reference material (RTC-CRM818-050), which was quantified using a standard addition protocol. Finally, the proposed HS-SPME-GC-microECD methodology was further applied to the screening of environmental soil samples for the presence of the target pesticides. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/18346746/Simultaneous_determination_of_traces_of_pyrethroids_organochlorines_and_other_main_plant_protection_agents_in_agricultural_soils_by_headspace_solid_phase_microextraction_gas_chromatography_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(08)00395-6 DB - PRIME DP - Unbound Medicine ER -