Abstract

In this work, a clean and simple magnetic solid-phase microextraction based on L-arginine modified magnetic dialdehyde starch nanocomposite was developed for the preconcentration and determination of diclofenac in biological samples by UV–Vis Spectrophotometry. A Plackett–Burman experimental design was used to evaluate the influence of effective parameters. Significant parameters were further optimized by Central Composite Design. Sample volume, pH and salting effect had a main effect on extraction of diclofenac by the proposed method. Under the optimized conditions, the detection limit (3 \({S}_{b}\), n = 7) was found to be 0.039 µg ml−1. The calibration curve showed dynamic linear 0.05–10 µg ml−1 with correlation coefficients (R2) of 0.987. The enrichment factor was found to be 148. The proposed method showed good results for preconcentration and determination of diclofenac in serum and pharmaceutical samples.

Highlights

  • IntroductionDiclofenac (DCF) is commonly used to relieve the symptoms of many diseases such as rheumatoid arthritis, osteoarthritis, spondylarthritis and ankylosing spondylitis [1, 2] and its global consumption is estimated to be around 940 tons per annum [3, 4] The chemical name is 2-[(2,6-dichlorophenyl)-aminophenyl]acetic acid (Fig. 1) and it belongs to the class of nonsteroidal anti-inflammatory drugs (NSAIDs), which is commonly used in different dosage and forms such as tablets, ointments or injections [5]

  • Diclofenac (DCF) is commonly used to relieve the symptoms of many diseases such as rheumatoid arthritis, osteoarthritis, spondylarthritis and ankylosing spondylitis [1, 2] and its global consumption is estimated to be around 940 tons per annum [3, 4] The chemical name is 2-[(2,6-dichlorophenyl)-aminophenyl]acetic acid (Fig. 1) and it belongs to the class of nonsteroidal anti-inflammatory drugs (NSAIDs), which is commonly used in different dosage and forms such as tablets, ointments or injections [5].During the last decade, consumption of pharmaceutical drug products has been increased to extremelevels [6] and because of their toxicity could pose threats to human health and the ecosystem

  • The resulting magnetic nanoparticles (MNPs) were characterized by Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM) and Vibrating sample magnetometer (VSM)

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Summary

Introduction

Diclofenac (DCF) is commonly used to relieve the symptoms of many diseases such as rheumatoid arthritis, osteoarthritis, spondylarthritis and ankylosing spondylitis [1, 2] and its global consumption is estimated to be around 940 tons per annum [3, 4] The chemical name is 2-[(2,6-dichlorophenyl)-aminophenyl]acetic acid (Fig. 1) and it belongs to the class of nonsteroidal anti-inflammatory drugs (NSAIDs), which is commonly used in different dosage and forms such as tablets, ointments or injections [5]. Chemometric calculations are cost-effective, useful, practical and efficient statistical approaches that can use for screening optimization of analytical procedures These methods provide several advantages such as the reagent consumption and analysis time reduction. The most relevant multivariate techniques used in analytical optimization is response surface methodology (RSM) that is based on Plackett-Burman Design (PBD), Central Composite Design (CCD) and Design of Experiment (DOE). It can be used for calculation of affective factors simultaneously more accurate combination and evaluation in permit assessment [24, 25]. Seven important factors including sample volume, salt effect, pH, amount of surfactant and sorbent, desorption and extraction time were selected to optimize

Material and instrumentation
Apparatus
Synthesis and characterization
Preparation of amine-functionalized MNPs
Modification of MNPs-NH2 by DAS and Arg
Statistical treatment of data
Characterization of MNPs-NH2 and Arg-MDAS
SEM analysis
Evaluation of method performance
Conclusion

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