Persistence and environmental implication of pharmaceuticals in agricultural soil is determined depending on adsorption, bioavailability and toxicity. This study aims to assess adsorption/partitioning behaviour of diclofenac (DCF) and its impact on microbial activity in four agricultural soils, differing in pH, organic carbon content, and cation exchange capacity. Results from batch studies suggests that soil/water partition coefficients of DCF are essentially nonlinear, i.e. depends on drug amount (p = 0.001), and positively correlated with soil organic carbon (p = 0.008). The adsorption data can effectively be modelled using Freundlich isotherm (regression coefficients between 0.84 and 0.90). In soil incubation studies, DCF could not be detected after 6 days of spiking (20 µg/g) in all soil types, including abiotic control. This suggests an interplay of combined biotic/abiotic process in DCF removal. Though microbial activity (based on tetrazolium reduction) declined with incubation time, but was not correlated with DCF exposure, particularly in soils rich in organic carbon.

Adsorption, Bioavailability and Microbial Toxicity of Diclofenac in Agricultural Soil.

A new, simple and reliable extractive-spectrophotometric method for the preconcentration and determination of diclofenac (DCF) was developed. In a strong nitric acid medium, diclofenac produced a yellowish compound in a water / tetrahydrofuran / perfluorooctanoic acid homogeneous phase that could be extracted into a sedimented microdroplet. The concentration of the extracted colored compound in the microdroplet was determined by measuring its absorbance at 376 nm. The effective experimental parameters for spectrophotometric determination of diclofenac in water and methanol were optimized, so that DCF could be sensitively determined in an aqueous or organic medium. The maximum absorbance was achieved in 1.5 and 7.0 M aqueous and methanolic solutions of nitric acid. The absorbance of DCF solutions in water and methanol obeyed Beer’s law, over the range of 1.0 - 30.0 µg cm-3 and 0.5 - 40.0 µg cm-3, with molar absorptivities of 7.4×10 3 and 1.3×10 4 dm 3 mol -1 cm -1 respectively. Additionally, different experimental parameters for homogeneous liquid-liquid extractions of diclofenac were investigated. The limit of detection (LOD) achieved with the proposed method was 0.03 ng cm-3. The maximum concentration factor obtained was 6667-fold. The reproducibility of 10 replicate measurements was found to be 2.3%. Finally, the proposed method was successfully applied to the extraction and determination of diclofenac in pharmaceutical preparations and urine samples.

A new homogeneous liquid-liquid extractive- spectrophotometric method for determination of diclofenac in urine

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A new homogeneous liquid-liquid extractive- spectrophotometric method for determination of diclofenac in urine