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Simple extraction method using syringe filter for detection of ethephon in tomatoes by negative‐ion mode liquid chromatography with tandem mass spectrometry
Authors:A M Abd El‐Aty  Md Musfiqur Rahman  Jeong‐Heui Choi  Young‐Jun Seo  Ho‐Chul Shin  Jae‐Han Shim
Institution:1. Biotechnology Research Institute, College of Agriculture and Life Sciences, Chonnam National University, Gwangju, Republic of Korea;2. Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, Giza, Egypt;3. Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Kwangjin‐gu, Seoul, Republic of Korea;4. National Agricultural Products Quality Management Service, Products Safety Inspection Laboratory, Gwangju, Republic of Korea
Abstract:In this study, a simple, rapid, and sensitive method was developed for the extraction of ethephon from homogenized tomatoes that does not require a cleanup procedure. In a syringe filter, three distinct layers – aqueous, acetonitrile, and n‐hexane – are clearly separated after storage at ?80 °C for 5–10 min. A Dionex IonPac column was used to separate the analyte before detection using negative‐ion mode liquid chromatography with tandem mass spectrometry (LC/MS/MS). The matrix effect of the tested analyte was negligibly small and the matched calibration showed a good linearity over a concentration range of 0.01–1.0 mg/kg with a correlation coefficient (R2) of 0.9998. The recovery at three fortification levels (0.1, 0.5 and 1.0 mg/kg) was between 82.9 and 108.6% with relative standard deviations (RSDs) <5.0%. The limit of quantification (0.03 mg/kg) was lower than the maximum residue limit (3 mg/kg) set by the Ministry of Food and Drug Safety, Republic of Korea. From a field trial, the method developed herein was applied to calculate the decline pattern and predict the pre‐harvest residue limits of ethephon in tomatoes. In conclusion, the proposed sample preparation is feasible for the detection of hydrophilic analytes in tomatoes. Copyright © 2015 John Wiley & Sons, Ltd.
Keywords:plant growth regulator  tomato  extraction  residue  tandem mass spectrometry  analysis  method validation
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