Rapid Analysis of 2,4-D in Soil Samples by Modified Soxhlet Apparatus Using HPLC with UV Detection

Abstract

The 2,4-dichlorophenoxy acetic acid (2,4-D) is used as a systemic herbicide to control broadleaf weeds in wheat, corn, range land/pasture land, sorghum, and barley. In this study, a fast and efficient method is developed by selection of modified extraction apparatus and high-performance liquid chromatography (HPLC)-UV conditions for the determination of 2,4-D in soil samples. The method is applied to the study of soil samples collected from the agricultural field. The herbicide is extracted from soil samples by acetonitrile in a modified Soxhlet apparatus. The advantages of the apparatus are that it uses small volume of organic solvent, reduced time of extraction, and better recovery of the analyte. The extract is filtered using a very fine microfiber paper. The total extract is concentrated in a rotatory evaporator, dried under ultrahigh pure N2, and finally reconstituted in 1 mL of acetonitrile. HPLC-UV at 228 nm is used for analysis. The herbicide is identified and quantitated using the HPLC system. The method is validated by the analysis of spiked soil samples. Recoveries obtained varied from 85% to 100% for spiked soil samples. The limit of quantitation (LOQ) and the limit of detection (LOD) are 0.010 and 0.005 parts per million (ppm), respectively, for spiked soil samples. The LOQ and LOD are 0.006 and 0.003 ppm for unspiked soil samples. The measured concentrations of 2,4-D in spiked soil samples are between 0.010 and 0.020 ppm with an average of 0.016 +/- 0.003 ppm. For unspiked soil samples it is between 0.006 ppm and 0.012 ppm with an average of 0.009 +/- 0.002 ppm. The measured concentrations of 2,4-D in soil samples are generally low and do not exceed the regulatory agencies guidelines.

Determination of 2,4-dichlorophenoxyacetic acid in water, sediment and soil using high performance liquid chromatography

“…The figures of merit of the Soxhlet method developed in the presented study for the determination of 2,4-D amine salt in water, sediment, and soil samples have been compared with other reported techniques [8,24]. Details of the relevant results of the methods and that of this study are provided in Tables 2 and 3.…”

“…The proposed method involves minimum labor and requires a short extraction time when compared to standard/tradition method. The performances of the developed technique were compared with that of the previously reported techniques of Kashyap et al [8] and Atalay and Hwang [24] in terms of relative recovery and regression coefficient (R 2 ). The findings confirmed that the developed technique is found to be comparable in terms of percent recoveries.…”

“…One of the most widely used herbicides in the cultivation today for the broadleaf weed control is 2,4-D either in acidic or in its amine salt form. It is classified as a phenoxyalkane acid [8]. Due to their high toxicity to dicotyledonous plants and low toxicity to monocotyledonous plants, 2,4-D herbicides are often used as selective herbicides Stella James et al…”

“…2023, 37 (2) 252 [9,10]. Apart from their usage as herbicides, these compounds are often used in high-input farming as seedless fruit germination promoters, defoliating agents, and typically as hormone growth regulators [8]. It has been reported that 2,4-D is usually used due to its limited persistence period, low-cost, and well-understood aquatic dynamics.…”

Determination of 2,4-Dichlorophenoxyacetic acid (2,4-D) in rat serum for pharmacokinetic studies with a simple HPLC method

“…High-performance liquid chromatography (HPLC) is general and popular for the analysis of drug and pesticide in biological samples [ 8 , 9 ]. Some HPLC methods have been established for the determination of 2,4-D residues in vegetables, fruits [ 10 ] and environmental samples [ 11 , 12 ], but only a few studies have been carried out for biological samples [ 13 , 14 ]. There is only limited data with respect to 2,4-D pharmacokinetic properties [ 15 ].…”