Rapid determination of 2,4-Dichlorophenoxyacetic acid residues in fruits by vortex-assisted derivatization and gas chromatography
Residues of 2,4-Dichlorophenoxyacetic acid (2,4-D) from agricultural use during the growth and transportation of fruits significantly affect their quality. To improve the detection efficiency of 2,4-D in fruits and while conserving energy and resources,a rapid detection method was developed using vortex-assisted derivatization combined with gas chromatography-electron capture detector (GC-ECD). Fruit samples were extracted with acetonitrile and dried under nitrogen. Subsequently,140 μL of methanol and 40 μL of concentrated sulfuric acid were added,and the mixture was vortexed for 1 minute to achieve rapid derivatization. Derivatives were extracted using n-hexane and purified with a saturated sodium chloride solution. Separation was performed on a DB-17 capillary column,and detection was achieved using GC-ECD. Quantification was conducted using both matrix-matched calibration curves and external standard method. The results demonstrated that 2,4-D exhibited good linearity in the range of 1.0～1000 μg/L with a correlation coefficient of 0.99993. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.001 and 0.003 mg/kg,respectively. Recover rates from spiking experiments ranged from 89.2％ to 103.8％,with relative standard deviations (RSDs) between 2.2％ and 6.2％. This method was simple to operate,had high detection efficiency,and compared to the current national standard method,reduced derivatization time by 44-fold,minimized reagent consumption,and shortened pretreatment time by 4～5 times. It is suitable for the rapid determination of 2,4-D residues in fruits.
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