Analytical study of trichlorfon residues in kaki fruit and cauliflower samples by liquid chromatography-electrospray tandem mass spectrometry
A detailed analytical study on trichlorfon residues in selected vegetables samples has been carried out, focused on the reliable quantification and confirmation of this compound, and on stability of residues under storage. As a consequence, a rapid and sensitive LC-ESI-MS/MS method has been developed for the determination of residues of this insecticide in kaki fruit (flesh and peel) and cauliflower samples. Extraction was performed with acetonitrile using a high-speed blender. After 4-fold dilution of the extract with water, 20 μL was directly injected in the LC-ESI-MS/MS system (triple quadrupole), using matrix-matched standards calibration for quantification. Under optimized MS/MS conditions, limit of detections between 0.006 and 0.013 mg/kg were reached, and a limit of quantification of 0.05 mg/kg was established, with a runtime of only 15 min. Recoveries from spiked blank samples at 0.05 and 0.5 mg/kg were in the range 83-101% with relative standard deviations lower than 10%. The method was applied to treated and untreated samples collected from field residues trials, using quality control samples analysis for the evaluation of the method. Despite the acquisition of two MS/MS transitions in selected reaction monitoring mode, the analysis of treated samples revealed the presence of a chromatographic peak close to the analyte that corresponded to a trichlorfon isobaric compound that shared the same MS/MS transitions. This unusual situation in LC-MS/MS-based procedures required the application of an efficient chromatographic separation to avoid this interference. All experiments have been made in compliance with the principles of Good. Laboratory Practices (GLP) and following the European SANCO guidelines for pesticides residue analysis (PRA). © 2006 American Chemical Society.
| Main Authors: | , , , , , |
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| Format: | artículo biblioteca |
| Language: | English |
| Published: |
American Chemical Society
2006
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| Subjects: | Trichlorfon, Pesticide residues, Vegetable samples, Liquid chromatography, Tandem mass spectrometry, Triple quadrupole, |
| Online Access: | http://hdl.handle.net/20.500.12792/5174 http://hdl.handle.net/10261/292307 |
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| Summary: | A detailed analytical study on trichlorfon residues in selected vegetables samples has been carried out, focused on the reliable quantification and confirmation of this compound, and on stability of residues under storage. As a consequence, a rapid and sensitive LC-ESI-MS/MS method has been developed for the determination of residues of this insecticide in kaki fruit (flesh and peel) and cauliflower samples. Extraction was performed with acetonitrile using a high-speed blender. After 4-fold dilution of the extract with water, 20 μL was directly injected in the LC-ESI-MS/MS system (triple quadrupole), using matrix-matched standards calibration for quantification. Under optimized MS/MS conditions, limit of detections between 0.006 and 0.013 mg/kg were reached, and a limit of quantification of 0.05 mg/kg was established, with a runtime of only 15 min. Recoveries from spiked blank samples at 0.05 and 0.5 mg/kg were in the range 83-101% with relative standard deviations lower than 10%. The method was applied to treated and untreated samples collected from field residues trials, using quality control samples analysis for the evaluation of the method. Despite the acquisition of two MS/MS transitions in selected reaction monitoring mode, the analysis of treated samples revealed the presence of a chromatographic peak close to the analyte that corresponded to a trichlorfon isobaric compound that shared the same MS/MS transitions. This unusual situation in LC-MS/MS-based procedures required the application of an efficient chromatographic separation to avoid this interference. All experiments have been made in compliance with the principles of Good. Laboratory Practices (GLP) and following the European SANCO guidelines for pesticides residue analysis (PRA). © 2006 American Chemical Society. |
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