Method validation and monitoring of emamectin benzoate in mature banana fruit with peel and pulp through Liquid chromatography-Mass spectrometry/ Mass spectrometry (LC-MS/MS)

Abstract

Emamectin benzoate has been frequently used in the banana ecosystem to combat the damage of pseudostem weevil. Therefore, the present study was conducted to validate the method, to assess harvest time residues and monitor emamectin benzoate residues in mature banana peel and pulp samples through LC-MS/MS. The validated method was used to determine emamectin benzoate residue in market banana samples. The study used Waters Alliance LC and Acquity TQD with an electrospray ionization interface in the positive ion mode. An isocratic flow of 0.1% formic acid (HCOOH) in water and 0.1% HCOOH in acetonitrile (CH3CN) was utilised for separation. CH₃CN was utilised to extract emamectin benzoate residue from the samples, and a dispersive solid-phase extraction technique was used for subsequent cleanup. Linearity tests were performed with standard solutions containing 0.01 to 0.1 g mL^-1, with three replicates for each concentration. For mature banana peel & pulp and mature banana pulp matrices, satisfactory recoveries of 79.85 to 95.09% and 89.20 to 100.94%, respectively and high precision relative standard deviations of 0.56 to 2.34% and 2.33 to 6.88%, respectively were obtained. For mature banana (peel and pulp, pulp alone) fruits, the lower detection and quantification limits were (0.003, 0.008), and (0.002, 0.007). The validated approach was utilised to analyse mature banana fruit samples obtained from emamectin benzoate treated fields and banana samples purchased from the local market.  Results showed satisfactory validation of parameters like linearity, the limit of detection and quantification, and recovery for determining emamectin benzoate residues in banana fruit.