Simultaneous Determination of Fluoroquinolones and Sulfonamides Originating from Sewage Sludge Compost

Abstract

A simultaneous method for quantitative determination of traces of fluoroquinolones (FQs) and sulfonamides (SAs) in edible plants fertilized with sewage sludge was developed. The compounds were extracted from the plants by rapid and simple liquid extraction followed by extracts clean-up using solid phase extraction. The eluent additive 1,1,1,3,3,3-hexafluoro-2-propanol was used for liquid chromatographic detection to achieve separation of structurally similar antimicrobials like ciprofloxacin and norfloxacin. Identification and quantification of the compounds were performed using high-performance liquid chromatography with electrospray ionization mass spectrometry in selected reaction monitoring mode. Method was validated and extraction recoveries of FQs and SAs ranged from 66% to 93%. The limit of quantifications was from 5 ng/g in the case of ofloxacin to 40 ng/g for norfloxacin. The method precision ranged from 1.43% to 2.61%. The developed novel method was used to evaluate the plats antimicrobial uptake (potato (Solanum tuberosum L.), carrot (Daucus carota L.), lettuce (Lactuca sativa L.), and wheat (Triticum vulgare L.)) from soil and migration of the analytes inside the plants.

Green and Efficient Determination of Fluoroquinolone Residues in Edible Green Fruits and Leafy Vegetables by Ultrasound-Assisted Extraction Followed by HPLC-MS/MS

“…However, the main challenge in the analysis of FQs in edible plants is related to their low concentration in vegetable tissues, and the presence of matrix components such as pigments, carbohydrates, and fatty or waxy materials can interfere in their determination [ 9 ]. The quantitative analysis can be performed by high-performance liquid chromatography equipped with fluorimetric detector (HPLC-FD) due to the high fluorescence of these compounds [ 16 , 17 ] and by high-performance liquid chromatography coupled with mass spectrometry detection (HPLC-MS/MS) [ 3 , 9 , 10 , 18 , 19 ], particularly recommended for complex matrices. Before instrumental quantitation, the sample preparation plays a key role in terms of analyte extraction, enrichment, and cleanup, but in most cases, it is a time-consuming and expensive step, and may contribute to further environmental problems mainly due to the quantities of hazardous wastes and the high energy demand.…”

“…However, the few methods currently proposed for FQ determination in vegetable matrices make use of prolonged extraction steps, mainly by ultrasound-assisted extraction (UAE) [ 9 , 10 , 12 , 20 ] and QuEChERS [ 2 , 15 , 21 ], by means of organic solvents such as acetonitrile (ACN), methanol (MeOH), acetone, hexane and chloroform. After the extraction, a cleanup step is usually performed, mostly by on-column solid-phase extraction (SPE) [ 9 , 12 , 18 , 19 ], dispersive SPE (d-SPE) [ 2 , 10 , 15 , 21 ] and liquid-liquid extraction (LLE) [ 20 ], which also require great amounts of organic solvents or sorbent material.…”

Optimization of a Method for Extraction and Determination of Residues of Selected Antimicrobials in Soil and Plant Samples Using HPLC-UV-MS/MS

“…The most commonly used are solid-liquid extraction (SLE) [25], ultrasound assisted extraction (UAE) [28] and pressurized liquid extraction (PLE) [29,30] combined with sample purification and pre-concentration using solid phase extraction (SPE) [17,[31][32][33][34]. High-performance liquid chromatography combined with a tandem mass spectrometer (HPLC-MS/MS) [17,32,33,35] is most often used to determine selected analytes in environmental samples, due to its high sensitivity and selectivity. The use of ultraviolet (UV) and fluorimetric detectors for the analysis of environmental samples is much less common, due to the low concentration range of antibiotics in the environment [36,37].…”

Penicillin biosensor based on rhombus‐shaped porous carbon/hematoxylin/penicillinase

“…At present, many practical and effective methods have been adopted to detect β‐lactam antibiotics within the food industry and animal husbandry, such as liquid chromatography (HPLC) (Samanidou et al., 2007), liquid chromatography‐mass spectrometry (LC‐MS) (Kipper et al., 2017), enzyme‐linked immunosorbent assay (ELISA) (Font et al., 2008; Zhao et al., 2007), and microbial detection methods (Myllyniemi et al., 2002). However, these methods are time‐consuming, expensive, environmentally demanding, and require complex sample preparation (Dey et al., 2005; Gramse & Jacobson, 2005; Picó & Barceló, 2008).…”