Quantitative Determination of Fluoroquinolones in Contaminated Soils by HPLC with Solid-Phase Extraction

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.

Synthesis of Molecularly Imprinted Polymers for Selective Extraction Followed by Solid Phase Determination of Metformin in Pharmaceutical Preparation and in Human Serum

“…-Solid phase extraction (SPE) is a technique designed for rapid, selective sample preparation and purification prior to the chromatographic analysis (e.g. HPLC(high performance liquid chromatography) , GC( gas chromatography), TLC(thin layer chromatography)) 13,14 . In SPE, one or more analytes from a liquid sample are isolated by extracting, partitioning, and adsorbing onto a solid stationary phase, Fig.…”

Investigation of 29 Antimicrobial Compounds in Soil Using Newly Developed UHPLC-MS/MS Method

“…As was previously described, manure-based organic fertilisers may be contaminated with VMPs, including antimicrobial agents and/or their metabolites [ 3 , 9 , 10 , 11 ]. Many authors report soil contamination with antimicrobial compounds caused by the use of organic manure-based fertilisers or wastewater from animal husbandry [ 3 , 4 , 10 , 11 , 12 , 13 , 14 , 15 ]. Moreover, we can also find researches describing crop contamination with antibiotics caused by the use of organic manure-based fertilisers [ 11 , 16 , 17 , 18 , 19 ].…”

“…Several multi-component methods are available in the literature for the determination of various veterinary antimicrobial drugs in soil [ 3 , 10 , 11 , 12 , 13 , 14 , 31 , 32 , 33 , 34 , 35 , 36 , 37 , 38 ]. Most of them enable the determination of only one class of compounds [ 14 , 37 ] or one substance from different xenobiotic classes [ 38 ] or up to four different classes [ 10 , 11 , 12 , 13 , 32 , 33 ]; only a few of them enable the determination of many substances from different classes [ 35 , 36 ]. Frequently, the isolation of analytes is based on liquid–solid extraction (LSE) coupled with solid-phase extraction (SPE) using one [ 3 , 12 , 13 , 14 , 32 , 38 ] or a combination of two different cartridges [ 10 , 35 ].…”

“…Most of them enable the determination of only one class of compounds [ 14 , 37 ] or one substance from different xenobiotic classes [ 38 ] or up to four different classes [ 10 , 11 , 12 , 13 , 32 , 33 ]; only a few of them enable the determination of many substances from different classes [ 35 , 36 ]. Frequently, the isolation of analytes is based on liquid–solid extraction (LSE) coupled with solid-phase extraction (SPE) using one [ 3 , 12 , 13 , 14 , 32 , 38 ] or a combination of two different cartridges [ 10 , 35 ]. Most of the methods are based on LC-MS/MS (liquid chromatography-tandem mass spectrometry) analysis [ 3 , 10 , 13 , 35 , 38 ].…”

“…Several multi-component methods are available in the literature for the determination of various veterinary antimicrobial drugs in soil [3,[10][11][12][13][14][31][32][33][34][35][36][37][38]. Most of them enable the determination of only one class of compounds [14,37] or one substance from different xenobiotic classes [38] or up to four different classes [10][11][12][13]32,33]; only a few of them enable the determination of many substances from different classes [35,36].…”