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

Abstract

The residues of antimicrobials used in human and veterinary medicine are popular pollutants of anthropogenic origin. The main sources of introducing antimicrobials into the environment are sewage treatment plants and the agricultural industry. Antimicrobials in animal manure contaminate the surrounding soil as well as groundwater, and can be absorbed by plants. The presence of antimicrobials in food of plant origin may pose a threat to human health due to their high biological activity. As part of the research, a procedure was developed for the extraction and determination of ciprofloxacin, enrofloxacin, cefuroxime, nalidixic acid and metronidazole in environmental samples (soil and parsley root). An optimized solid-liquid extraction (SLE) method was used to separate antimicrobials from the solid samples and a mixture of citrate buffer (pH = 4): methanol (1:1; v/v) was used as the extraction solvent. Solid phase extraction (SPE) with OASIS® HLB cartridges was used to purify and pre-concentrate the sample. The recovery of the developed method was in the range of 55–108%. Analytes were determined by high-performance liquid chromatography coupled with an ultraviolet (UV) detector and a tandem mass spectrometer (HPLC-UV-MS/MS). The procedure was validated and applied to the determination of selected antimicrobials in soil and parsley root samples. Five types of soil and five types of parsley roots of different origins were analyzed. The presence of nalidixic acid in the parsley root samples was found in the concentration range of 0.14–0.72 ng g−1. It has been shown that antimicrobials are absorbed by the plant and can accumulate antimicrobials in its edible parts.

Uptake of Pharmaceutical Pollutants and Their Metabolites from Soil Fertilized with Manure to Parsley Tissues

“…SLE-SPE extraction of five selected FCs from parsley root has already been studied by our research team [ 38 ]. In the present study, the SLE-SPE procedure was also used to extract 14 selected analytes, and the SLE step was modified.…”

“…Reports have shown that the most common elution of analytes from HLB sorbent after passing the plant matrix extract is carried out under inert conditions-MeOH [6,9], although our study indicated that sequential elution with solvents of different pH gave a higher recovery of FCs. [38]. In the present study, the SLE-SPE procedure was also used to extract 14 selected analytes, and the SLE step was modified.…”

“…The efficiency of SLE-SPE L5 extraction was low for the other 6 analytes (SMX, SFD, MET, TRI, TYL, CLR), so it was necessary to use a procedure based on double SLE extraction with MeOH for their separation (SLE L1, without using SPE; recoveries 61.9-89.9%).3.1.4. Parsley Root-Development of SLE-SPE ProcedureSLE-SPE extraction of five selected FCs from parsley root has already been studied by our research team[38]. In the present study, the SLE-SPE procedure was also used to extract 14 selected analytes, and the SLE step was modified.…”

Determination of multiple antibiotics in agricultural soil using a quick, easy, cheap, effective, rugged, and safe method coupled with ultra‐high performance liquid chromatography‐tandem mass spectrometry

“…According to past studies, mixing organic acids (including formic acid [39], phosphate [41], Na 2 EDTA-Mcllvaine [38,42]) with methanol [37] or ACN [43] is the most effective extraction solution with good recovery efficiency and has good reproducibility when analyzing multiple antibiotic residues in environmental matrices. Ferhi et al [34] demonstrated that ACN and citric acid-phosphate buffer can be used to efficiently extract eight antibiotics from the soil.…”

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

“…However, AMs are not completely metabolized and a fraction between 17% and 90% is excreted unchanged in urine and feces, leading to notably widespread contamination of water and soil resources. AMs may enter agricultural fields mainly via the use of recycled water for irrigation due to the incomplete removal of these pharmaceuticals in wastewater treatment processes, and land application of sewage sludge, biosolids and manure as soil amendments or fertilizers instead of chemical fertilizers, which are restricted for organic vegetables [ 1 , 2 , 3 , 4 , 5 , 6 , 7 , 8 , 9 , 10 , 11 , 12 ].…”