scholarly journals Simultaneous Determination of Six Triazolic Pesticide Residues in Apple and Pear Pulps by Liquid Chromatography with Ultraviolet Diode Array Detection

2001 ◽  
Vol 84 (5) ◽  
pp. 1543-1550 ◽  
Author(s):  
Carlo Bicchi ◽  
Chiara Cordero ◽  
Patrizia Rubiolo ◽  
Alessandro Occelli

Abstract A method is described for the simultaneous determination of diclobutrazol, flusilazole, flutriafol, hexaconazole, paclobutrazol, and tetraconazole in apple and pear pulps used in baby food at a limit of 0.01 mg/kg. Apple and pear pulp samples are subjected to selective solid-phase microdispersion (SPMD) with SPE-ED Matrix-38 and acetone–cyclohexane, and the extracts are cleaned up on a Florisil cartridge with hexane–cyclohexane–acetone. The extracts are then analyzed by liquid chromatography with ultraviolet detection, using an octadecylsilane column with a gradient-programmed acetonitrile–water mobile phase. Recoveries were determined by spiking apple and pear pulps with the 6 pesticides under investigation at 0.1, 0.05, 0.03, and 0.01 mg/kg. Six determinations were performed at each level for each pesticide. Recoveries were ≥70% at the 0.01 mg/kg level.

2017 ◽  
Vol 2017 ◽  
pp. 1-5 ◽  
Author(s):  
Antonella Aresta ◽  
Pietro Cotugno ◽  
Federica Massari ◽  
Carlo Zambonin

A new analytical method, based on liquid chromatography (LC) with UV-diode array detection, for the simultaneous determination of daidzein, genistein, and glycitein and their 7-O-β-D-glucopyranoside (daidzin, genistin, and glycitin, resp.) has been successfully developed. All the calibration curves showed good linearity within the concentration range 0.02–2 μg/ml. The limits of detection and quantitation were 0.057 (genistin and glycitein), 0.124 μg/ml (genistein), 0.190 μg/ml (genistin and glycitein), and 0.410 μg/ml (genistein), respectively. Within-day and between-days precision were found not to be significantly different according to an F-test; values (% RSD) ranged from 2.0 to 2.9%. Extraction and clean-up of soybean flour samples were carried out using matrix solid-phase dispersion extraction (MSPD). The main parameters affecting extraction yield, such as dispersant, type and amount of additives, cosorbent, and extractive solvent, were evaluated and optimized. The average recovery values were between 85.7 and 102.6%. The target isoflavone concentration levels estimated in this work fit existing literature data and were comprised between 39.3 and 345.3 μg/g. The whole procedure has proved to be simple, accurate, precise, and cheap.


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