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Large-scale pesticide testing in olives by liquid chromatography-electrospray tandem mass spectrometry using two sample preparation methods based on matrix solid-phase dispersion and QuEChERS.
J Chromatogr A. 2010 Sep 24; 1217(39):6022-35.JC

Abstract

In this work we have evaluated the performance of two sample preparation methodologies for the large-scale multiresidue analysis of pesticides in olives using liquid chromatography-electrospray tandem mass spectrometry (LC-MS/MS). The tested sample treatment methodologies were: (1) liquid-liquid partitioning with acetonitrile followed by dispersive solid-phase extraction clean-up using GCB, PSA and C18 sorbents (QuEChERS method - modified for fatty vegetables) and (2) matrix solid-phase dispersion (MSPD) using aminopropyl as sorbent material and a final clean-up performed in the elution step using Florisil. An LC-MS/MS method covering 104 multiclass pesticides was developed to examine the performance of these two protocols. The separation of the compounds from the olive extracts was achieved using a short C18 column (50 mm x 4.6 mm i.d.) with 1.8 microm particle size. The identification and confirmation of the compounds was based on retention time matching along with the presence (and ratio) of two typical MRM transitions. Limits of detection obtained were lower than 10 microgkg(-1) for 89% analytes using both sample treatment protocols. Recoveries studies performed on olives samples spiked at two concentration levels (10 and 100 microgkg(-1)) yielded average recoveries in the range 70-120% for most analytes when QuEChERS procedure is employed. When MSPD was the choice for sample extraction, recoveries obtained were in the range 50-70% for most of target compounds. The proposed methods were successfully applied to the analysis of real olives samples, revealing the presence of some of the target species in the microgkg(-1) range. Besides the evaluation of the sample preparation approaches, we also discuss the use of advanced software features associated to MRM method development that overcome several limitations and drawbacks associated to MS/MS methods (time segments boundaries, tedious method development/manual scheduling and acquisition limitations). This software feature recently offered by different vendors is based on an algorithm that associates retention time data for each individual MS/MS transition, so that the number of simultaneously traced transitions throughout the entire chromatographic run (dwell times and sensitivity) is maximized.

Authors+Show Affiliations

Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Campus Las Lagunillas, Edificio B-3, 23071 Jaén, Spain.No 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

20728894

Citation

Gilbert-López, Bienvenida, et al. "Large-scale Pesticide Testing in Olives By Liquid Chromatography-electrospray Tandem Mass Spectrometry Using Two Sample Preparation Methods Based On Matrix Solid-phase Dispersion and QuEChERS." Journal of Chromatography. A, vol. 1217, no. 39, 2010, pp. 6022-35.
Gilbert-López B, García-Reyes JF, Lozano A, et al. Large-scale pesticide testing in olives by liquid chromatography-electrospray tandem mass spectrometry using two sample preparation methods based on matrix solid-phase dispersion and QuEChERS. J Chromatogr A. 2010;1217(39):6022-35.
Gilbert-López, B., García-Reyes, J. F., Lozano, A., Fernández-Alba, A. R., & Molina-Díaz, A. (2010). Large-scale pesticide testing in olives by liquid chromatography-electrospray tandem mass spectrometry using two sample preparation methods based on matrix solid-phase dispersion and QuEChERS. Journal of Chromatography. A, 1217(39), 6022-35. https://doi.org/10.1016/j.chroma.2010.07.062
Gilbert-López B, et al. Large-scale Pesticide Testing in Olives By Liquid Chromatography-electrospray Tandem Mass Spectrometry Using Two Sample Preparation Methods Based On Matrix Solid-phase Dispersion and QuEChERS. J Chromatogr A. 2010 Sep 24;1217(39):6022-35. PubMed PMID: 20728894.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Large-scale pesticide testing in olives by liquid chromatography-electrospray tandem mass spectrometry using two sample preparation methods based on matrix solid-phase dispersion and QuEChERS. AU - Gilbert-López,Bienvenida, AU - García-Reyes,Juan F, AU - Lozano,Ana, AU - Fernández-Alba,Amadeo R, AU - Molina-Díaz,Antonio, Y1 - 2010/08/01/ PY - 2010/04/30/received PY - 2010/07/22/revised PY - 2010/07/23/accepted PY - 2010/8/24/entrez PY - 2010/8/24/pubmed PY - 2010/12/14/medline SP - 6022 EP - 35 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1217 IS - 39 N2 - In this work we have evaluated the performance of two sample preparation methodologies for the large-scale multiresidue analysis of pesticides in olives using liquid chromatography-electrospray tandem mass spectrometry (LC-MS/MS). The tested sample treatment methodologies were: (1) liquid-liquid partitioning with acetonitrile followed by dispersive solid-phase extraction clean-up using GCB, PSA and C18 sorbents (QuEChERS method - modified for fatty vegetables) and (2) matrix solid-phase dispersion (MSPD) using aminopropyl as sorbent material and a final clean-up performed in the elution step using Florisil. An LC-MS/MS method covering 104 multiclass pesticides was developed to examine the performance of these two protocols. The separation of the compounds from the olive extracts was achieved using a short C18 column (50 mm x 4.6 mm i.d.) with 1.8 microm particle size. The identification and confirmation of the compounds was based on retention time matching along with the presence (and ratio) of two typical MRM transitions. Limits of detection obtained were lower than 10 microgkg(-1) for 89% analytes using both sample treatment protocols. Recoveries studies performed on olives samples spiked at two concentration levels (10 and 100 microgkg(-1)) yielded average recoveries in the range 70-120% for most analytes when QuEChERS procedure is employed. When MSPD was the choice for sample extraction, recoveries obtained were in the range 50-70% for most of target compounds. The proposed methods were successfully applied to the analysis of real olives samples, revealing the presence of some of the target species in the microgkg(-1) range. Besides the evaluation of the sample preparation approaches, we also discuss the use of advanced software features associated to MRM method development that overcome several limitations and drawbacks associated to MS/MS methods (time segments boundaries, tedious method development/manual scheduling and acquisition limitations). This software feature recently offered by different vendors is based on an algorithm that associates retention time data for each individual MS/MS transition, so that the number of simultaneously traced transitions throughout the entire chromatographic run (dwell times and sensitivity) is maximized. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/20728894/Large_scale_pesticide_testing_in_olives_by_liquid_chromatography_electrospray_tandem_mass_spectrometry_using_two_sample_preparation_methods_based_on_matrix_solid_phase_dispersion_and_QuEChERS_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(10)00998-2 DB - PRIME DP - Unbound Medicine ER -