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Fluorescence

Determination of Kresoxim-Methyl in Water and in Grapes by High-Performance Liquid Chromatography (HPLC) Using Photochemical-Induced Fluorescence and Dispersive Liquid-Liquid Microextraction (DLLME)

, , , , , & show all
Pages 2202-2221 | Received 21 Oct 2019, Accepted 19 Feb 2020, Published online: 06 Mar 2020
 

Abstract

A high-performance chromatographic method was developed to determine the fungicide kresoxim-methyl. Off-line photochemical derivatization was used to induce the formation of a stable and fluorescent product since the fungicide does not present natural fluorescence. Intense fluorescence at 370/430 nm was achieved by treating the analyte in solution at pH 6 to ultraviolet light for 45 s. The chromatographic conditions included isocratic elution with 50/50% (v/v) acetonitrile/water and the photochemical product appeared at a retention time of 7.2 min. The short and long term stabilities of the photoproduct were evaluated and variation of less than 5% was achieved. The limits of detection in water samples and in grapes samples were 0.019 mg kg−1 and 0.065 mg kg−1 of kresoxim- methyl residue, respectively. The linear response covered three orders of magnitude up to 10.6 mg kg−1 of kresoxim-methyl. The robustness was evaluated through a Box–Behnken experimental design showing the insignificance of all factors and their interactions. The potential interference of tebuconazole for the determination of kresoxim-methyl was studied. The use of the dispersive liquid-liquid microextraction (DLLME) allowed recoveries between 80% and 101% depending on concentration with the minimum generation of waste products.

Acknowledgments

Cunha, Macedo, and Lamounier are grateful to Dr. Isabelle Karine da Costa Nunes (LADETEC/IQ, UFRJ) for analyses carried out to identify the photo-products.

Disclosure statement

No potential conflict of interest was reported by the author(s).

Additional information

Funding

Cunha, Macedo, and Lamounier thank IFRJ/CNPq for support and scholarship (Prociency/PIBIC). Silva thanks the IFRJ scholarship (PIBIC). Aucelio thanks the Brazilian scientific agencies CNPq (303866/2017-9) and FAPERJ (E-26/202.912/2017) for research grants and scholarships. Almeida thanks CNPq for scholarship (141.071/2014-1) and Toloza acknowledges his FAPERJ scholarship (E-26/200.435/2016).

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