Simple extraction method using syringe filter for detection of ethephon in tomatoes by negative-ion mode liquid chromatography with tandem mass spectrometry

• Published in: Biomedical chromatography Vol. 29; no. 10; pp. 1480 - 1485
• Main Authors: Cho, Soon-Kil, Cho, Ji-Mi, Abd El-Aty, A. M., Rahman, Md. Musfiqur, Choi, Jeong-Heui, Seo, Young-Jun, Shin, Ho-Chul, Shim, Jae-Han
• Format: Journal Article
• Language: English
• Published: England Blackwell Publishing Ltd 01.10.2015
• Subjects: analysis; Calibration; Chemical Fractionation - instrumentation; Chemical Fractionation - methods; Chromatography, Liquid - methods; Equipment Design; extraction; Food Analysis - methods; Half-Life; Limit of Detection; Lycopersicon esculentum - chemistry; Lycopersicon esculentum - drug effects; method validation; Organophosphorus Compounds - analysis; Organophosphorus Compounds - pharmacology; plant growth regulator; Reproducibility of Results; residue; tandem mass spectrometry; Tandem Mass Spectrometry - methods; tomato; method validation; plant growth regulator; tandem mass spectrometry; tomato; analysis; extraction; residue
• ISSN: 0269-3879; 1099-0801
• DOI: 10.1002/bmc.3446

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.