Liquid chromatography/atmospheric pressure chemical ionization-mass spectrometric analysis of benzoylurea insecticides in citrus fruits
2000; Wiley; Volume: 14; Issue: 7 Linguagem: Inglês
10.1002/(sici)1097-0231(20000415)14
ISSN1097-0231
AutoresA. I. Valenzuela, Y. Pic�, Guillermina Font,
Tópico(s)Pesticide Residue Analysis and Safety
ResumoRapid Communications in Mass SpectrometryVolume 14, Issue 7 p. 572-577 Research Article Liquid chromatography/atmospheric pressure chemical ionization-mass spectrometric analysis of benzoylurea insecticides in citrus fruits A. I. Valenzuela, A. I. Valenzuela Laboratori de Toxicologia, Facultat de Farmàcia, Universitat de València, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, València, SpainSearch for more papers by this authorY. Picó, Y. Picó Laboratori de Toxicologia, Facultat de Farmàcia, Universitat de València, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, València, SpainSearch for more papers by this authorG. Font, Corresponding Author G. Font [email protected] Laboratori de Toxicologia, Facultat de Farmàcia, Universitat de València, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, València, SpainLaboratori de Toxicologia, Facultat de Farmácia, Universitat de Valéncia, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, Valéncia, SpainSearch for more papers by this author A. I. Valenzuela, A. I. Valenzuela Laboratori de Toxicologia, Facultat de Farmàcia, Universitat de València, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, València, SpainSearch for more papers by this authorY. Picó, Y. Picó Laboratori de Toxicologia, Facultat de Farmàcia, Universitat de València, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, València, SpainSearch for more papers by this authorG. Font, Corresponding Author G. Font [email protected] Laboratori de Toxicologia, Facultat de Farmàcia, Universitat de València, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, València, SpainLaboratori de Toxicologia, Facultat de Farmácia, Universitat de Valéncia, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, Valéncia, SpainSearch for more papers by this author First published: 27 April 2000 https://doi.org/10.1002/(SICI)1097-0231(20000415)14:7 3.0.CO;2-2Citations: 32Read the full textAboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onEmailFacebookTwitterLinkedInRedditWechat Abstract A liquid chromatography (LC) method for the quantitative determination of three benzoylurea insecticide residues (diflubenzuron, flufenoxuron and hexaflumuron) in citrus fruits is described. Residues were successfully separated on a C18 column by methanol/water gradient elution. Detection was by negative-ion, selected-ion monitoring atmospheric pressure chemical ionization-mass spectrometry (APCI-MS); the main ions were [M − H]−, and the secondary fragment ions were [M − H − HF]−. Useful confirmatory information can thus be obtained at low extraction voltages from losses of HF. Detection limits for standard solutions were 10 fg injected and good linearity and reproducibility were obtained. The optimum LC/APCI-MS conditions were applied to the analysis of benzoylureas in oranges. Samples were extracted using matrix solid phase dispersion (MSPD), in which orange samples were homogenized with C8, placed onto a glass column and eluted with dichloromethane. Detection limits of 2 µg kg−1 in the crop were obtained. Average recoveries from citrus fortified with approximately (25–1000 µg kg−1) ranged from 87 to 102%. 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