Abstract
This work reports the development of an analytical method for the simultaneous analysis of three fluoroquinolones; ciprofloxacin (CIP), norfloxacin (NOR) and ofloxacin (OFL) in soil matrix. The proposed method was performed by using microwave-assisted extraction (MAE), solid-phase extraction (SPE) for samples purification, and finally the pre-concentrated samples were analyzed by HPLC detector. In this study, various organic solvents were tested to extract the test compounds, and the extraction performance was evaluated by testing various parameters including extraction solvent, solvent volume, extraction time, temperature and number of the extraction cycles. The current method showed a good linearity over the concentration ranging from 1 – 300ng g-1 with correlation coefficients (r2 > 0.998) for all test compounds. Good recoveries were also obtained for the test compounds ranged from 89 – 99 %. The relative standard deviation (RSD) from intra-day and inter-day precision was lower than 7%, and the detection (LOD) and quantification (LOQ) limits ranged from 0.9 – 2.7ng g-1.Finally, the proposed method was applied to determine the target compounds in real soil samples irrigated with wastewater. The results confirm the presence of the test compounds in soils with values ranging from 1.9 – 4.6ng g-1, as well as the suitability of the proposed method to determine the test compounds in real soil matrix as well as the ability of the test compounds to accumulate in soils irrigated with sewage.
Highlights
Pharmaceuticals are the most common practice for human treatment and/or prevention of illness
To evaluate the performance of extraction technique to isolate the test compounds from soil matrix, several parameters influencing the microwave-assisted extraction (MAE) performance should be taken in consideration
Since the fluoroquinolones have a tendency to form complexes with metal ions reducing the extraction efficiency, Na2EDTA was added to samples to avoid test compound bonding with metal residues in the sample which reduce the extraction efficiency [25, 26, 27]
Summary
Pharmaceuticals are the most common practice for human treatment and/or prevention of illness. The chemical structure of fluoroquinolones is derived from quinolone which has a bicycle structure with nitrogen, carboxylic acid and carbonyl groups in positions 1, 3 and 4, respectively. In addition to these functional groups, fluoroquinolones contain fluorine in position 7 which contributes to carboxylic group in polar character of fluoroquinolones (log Kow between -1.03 to 0.89). The presence of ketone, hydroxyl group and amid in fluoroquinolones structure making it able to form complexes with many of divalent and trivalent cations such as Mg2+, Ca2+, and Al3+ which make fluoroquinolones capable of being adsorbed on soil clay surface [8,9]
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