Development and Method Validation for the Analysis of Ethephon Residues in Fruits Using Headspace Gas Chromatography–Mass Spectrometry
Keywords:
Pesticide residues, Ethephon, Ethylene, Fruits, Gas chromatography–mass spectrometryAbstract
Ethephon is a plant growth regulator widely used during postharvest handling to accelerate fruit ripening. In this study, tropical fruits including banana, mango, pineapple, and durian, as well as temperate fruits including apple, cherry, and strawberry, were investigated. Improper use of ethephon may result in residue contamination and potential risks to consumer safety. This study aimed to develop and validate a method for the determination of ethephon residues in fruits based on the alkaline decomposition of ethephon to generate ethylene gas, followed by analysis using headspace–gas chromatography–mass spectrometry (HS–GC–MS). The developed method demonstrated high selectivity, with ethylene detected at a retention time of 2.45 min and characteristic ions at m/z 27, 26, and 28. No interfering peaks were observed in the method blank, while naturally occurring ethylene in all fruit matrix blanks was detected below the limit of detection (LOD). Quantification was performed using external calibration because matrix effects were low and statistically insignificant. Linearity was achieved within the range of 0.1–4.0 µg (R2 = 1.0000), while matrix calibration curves showed R2 values of 0.9986–0.9998. The LOD and limit of quantitation (LOQ) values for tropical fruits were 0.10 and 0.30 mg/kg, respectively, whereas those for temperate fruits were 0.02 and 0.05 mg/kg, respectively. Tropical fruits showed recoveries of 81.4–119.0% with %RSD values of 1.5–16.0, while temperate fruits showed recoveries of 89.8–120.0% with %RSD values of 2.9–13.9. Overall, the developed HS–GC–MS method was accurate, reliable, and suitable for confirmatory determination of ethephon residues in fruits.
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