A Rapid and Sensitive Single Residual Method for Determination of Ethephon in Grape by high performance liquid chromatography-tandem mass spectrometry/ Um método residual rápido e sensível para a determinação de Ethephon em uvas por cromatografia líquida de alta eficiência e espectrometria de massa em tandem

Anna Luiza Brito de Souza, Jessyca Wanessa Soares Araujo Silva, Henrique Carlos Marinho Pereira Silva, Analucia Guedes Silveira Cabral, Clayton Anderson de Azevedo Filho, Ellison Neves de Lima, Carlos Eduardo Miranda de Sousa

Abstract


This paper describes a rapid (7.0 min) and sensitive (LLOQ 0.1 ng/mL) analytical method for the quantitation of Ethephon  in grape.  A new method for the detection and quantification of ETP residues in fruit and vegetables was developed. The present study indicates that fruit and vegetables require a rapid and simple cleanup step before using gas chromatograph/mass spectrometry. The recovery and precision of the new method were evaluated by spiking the fruit and vegetable samples with 0.01-0.1 μg/g of ETP. The method is based on High-performance Liquid chromatography-tandem mass spectrometry (LC-MS/MS).The chromatographic separation was achieved on a Hypercarb 2.1x 100 mm 5µm reversed-phase column and a mobile phase containing water/mathanol (97:3 v/v, add 1% acetic acid), in isocratic conditions. The target analytes were transferred into a triple quadrupole mass spectrometer equipped with an electrospray ionization source for mass detection. The ion transitions selected for MRM detection were:  m/z 142.8 >106.8, m/z 144.8 >106.8 and 106.8>78.8 for ETP. The linearity of the detector response was demonstrated in the range from 0.01 to 1 µg/g for each analyte with a coefficient of determination (R2) of ≥0.999. The method was successfully applied to determination of ethephon in bunch grapes from five free trade fairs in the city of Caruaru, Pernambuco, Brazil.


Keywords


Ethephon, LC-MS/MS, Grape, Validation

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References


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DOI: https://doi.org/10.34119/bjhrv2n6%20-005

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