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Development of an ultrasound‐assisted emulsification microextraction method for the determination of chlorpyrifos and organochlorine pesticide residues in honey samples using gas chromatography with mass spectrometry
Authors:Mir‐Michael Mousavi  Seyedrafie Arefhosseini  Ali Akbar Alizadeh Nabili  Mansour Mahmoudpour  Mahboob Nemati
Affiliation:1. Drug Applied Research Center, Tabriz University of Medical Sciences, Tabriz, Iran;2. Faculty of Nutrition, Tabriz University of Medical Sciences, Tabriz, Iran;3. Students’ Research Committee, Faculty of Nutrition, Tabriz University of Medical Sciences, Tabriz, Iran;4. Food and Drug control Laboratories, Tabriz University of Medical Sciences, Tabriz, Iran;5. Faculty of Pharmacy, Tabriz University of Medical Sciences, Tabriz, Iran
Abstract:A simple, rapid, and efficient ultrasound‐assisted emulsification microextraction method followed by gas chromatography mass spectrometry in selected ion monitoring mode was developed for the determination of organochlorine pesticides in honey samples. The type and volume of organic extraction solvent, pH, effect of added salt content, and centrifuging time and speed were investigated. Under the optimum extraction conditions, 30 μL of 1, 2‐dibromoethane (extraction solvent) was immersed into an ultrasonic bath for 1 min at 40°C. The limits of detection and quantification for all target pesticides were 0.003–0.06 and 0.01–0.2 ng/g, respectively. The extraction recovery was 91–100% and the enrichment factors were 168–192. The relative standard deviation for the method was <6% for intraday (n = 6) and <8% for interday precision (n = 4). The proposed method was successfully applied for the analysis of organochlorine pesticides in honey samples.
Keywords:Gas chromatography  Honey  Mass spectrometry  Pesticide residues  Ultrasound‐assisted emulsification microextraction
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