Determination of polyether ionophores in urban sewage sludge by pressurised liquid extraction and liquid chromatography–tandem mass spectrometry: Study of different clean-up strategies

• Published in: Journal of Chromatography A Vol. 1285; pp. 31 - 39
• Main Authors: Herrero, P., Borrull, F., Marcé, R.M., Pocurull, E.
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 12-04-2013; Elsevier
• Subjects: acetone; Analysis methods; Analytical chemistry; Applied sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography; Chromatography, Liquid - methods; Cleaning; detection limit; Exact sciences and technology; Extraction; Heterocyclic Compounds, 1-Ring - analysis; Heterocyclic Compounds, 1-Ring - chemistry; Heterocyclic Compounds, 1-Ring - isolation & purification; In-cell clean-up; Ionophores - analysis; Ionophores - chemistry; Ionophores - isolation & purification; Lactones - analysis; Lactones - chemistry; Lactones - isolation & purification; Limit of Detection; liquid chromatography; Liquid chromatography–tandem mass spectrometry; Liquid-Liquid Extraction - methods; Liquids; Matrix effect; Monensin; narasin; Other chromatographic methods; Other industrial wastes. Sewage sludge; Pollution; Polyether ionophores; Polymers - analysis; Polymers - chemistry; Polymers - isolation & purification; Pressurised liquid extraction; Reproducibility of Results; Sewage - chemistry; Sewage sludge; sewage treatment; Sludge; solid phase extraction; Spain; Strategy; tandem mass spectrometry; Tandem Mass Spectrometry - methods; Waste Management; Wastes; Water Pollutants, Chemical - analysis; Water Pollutants, Chemical - chemistry; Water Pollutants, Chemical - isolation & purification; Spain; Spain, Catalonia; Pressurised liquid extraction; Matrix effect; Polyether ionophores; Sewage sludge; In-cell clean-up; Liquid chromatography–tandem mass spectrometry; Solid phase extraction; Tandem mass spectrometry; Chemical analysis; HPLC chromatography; Liquid chromatography-tandem mass spectrometry; Solvent extraction; Electrospray; Chemical enrichment; Acetal; Antiprotozoal agent; Antifungal agent; Sample preparation; Ionophore; Quantitative analysis; Lasalocid; Ether; Monensin; Coupled method; Operating conditions; Antibiotic; Reversed phase chromatography; Pressure effect; Salinomycin; Narasin; Maduramicin; Parasiticide; Antibacterial agent
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2013.02.034

► Several clean-up strategies to reduce the matrix effect in sewage sludge extracts were studied. ► Pressurised liquid extraction provides recoveries up to 90% for all compounds. ► Developed method provides limits of detection and quantification at low μg/kg (d.w.). ► Monensin and narasin were determined in sewage sludge for the first time.
A method for the determination of five polyether ionophores in urban sewage sludge has been developed. The extraction of compounds was performed by pressurised liquid extraction using acetone, while florisil was used for in-cell clean-up to minimise the matrix effect in the sludge extracts. An amide polar-embedded reversed-phase column was used for the chromatographic separation with a rapid-resolution liquid chromatograph coupled to a tandem mass spectrometer. Moreover, several clean-up strategies such as in-cell and on-cell clean-up and solid-phase extraction clean-up, among others, were tested and their results are discussed in the present paper. Recoveries (10 and 250μg/kg in dry weight (d.w.), n=6) were close to 90%, repeatability and reproducibility (%RSD, 10 and 250μg/kg (d.w.), n=6) were less than 10% and12%, respectively. Limits of detection (LODs) and limits of quantification (LOQs) ranged between 0.5 and 1μg/kg (d.w.) and between 1 and 5μg/kg (d.w.), respectively. The method was applied to samples collected in five sewage treatment plants in Catalonia. Monensin and narasin were determined in some sludge samples at concentrations from <LOQ to 3.5μg/kg (d.w.) for monensin and from <LOQ to 3.7μg/kg (d.w.) for narasin.