title: Development of a rapid method for the determination and confirmation of nitroimidazoles in six matrices by fast liquid chromatography-tandem mass spectrometry.
abstract: A rapid liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed to identify and to quantify nitroimidazoles, metronidazole (MNZ), ronidazole (RNZ) and dimetridazole (DMZ) and their corresponding hydroxy metabolites, MNZ-OH and 2-hydroxymethyl-1-methyl-5-nitroimidazole (HMNNI) in plasma, milk, muscle, egg, honey and feed samples. The same sample clean-up procedure including a novel solid-phase extraction (SPE) on polymeric Strata-SDB cartridges was used for each matrix. The analytes were separated on Kinetex XB C-18 core-shell type HPLC column using isocratic elution mode with a mobile phase containing 0.1% formic acid in water/methanol (88/12, v/v, pH 2.6) at a flow rate of 0.7 ml/min. The main advantage of the developed method is that the analysis time of only 3 min, which is about three to ten times shorter than in other reported HPLC methods. The developed method was validated using a matrix-comprehensive in-house validation strategy. The matrix effect of LC-MS/MS analysis was also investigated. Results are presented from the successful application of the developed method to an incurred pork meat certified reference material and to incur porcine plasmas in a proficiency test in year 2011.
authors.affiliation: Central Agricultural Office Food and Feed Safety Directorate, Food Toxicological National Reference Laboratory, Mester utca 81, Budapest, Hungary. adam.tolgyesi@t-online.hu
authors.forename: Adám
authors.initials: A
authors.lastname: Tölgyesi
authors.forename: Virender K
authors.initials: VK
authors.lastname: Sharma
authors.forename: Szabolcs
authors.initials: S
authors.lastname: Fekete
authors.forename: Jenő
authors.initials: J
authors.lastname: Fekete
authors.forename: Andrea
authors.initials: A
authors.lastname: Simon
authors.forename: Szilvia
authors.initials: S
authors.lastname: Farkas
mesh_terms: D000821:Animal Feed / Q000032:analysis; D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004131:Dimetridazole / Q000031:analogs & derivatives / Q000032:analysis* / Q000097:blood / Q000737:chemistry; D004350:Drug Residues / Q000032:analysis*; D004531:Eggs / Q000032:analysis; D006722:Honey / Q000032:analysis; D008460:Meat / Q000032:analysis; D008795:Metronidazole / Q000031:analogs & derivatives / Q000032:analysis* / Q000097:blood / Q000737:chemistry; D008892:Milk / Q000737:chemistry; D015394:Molecular Structure; D009132:Muscles / Q000737:chemistry; D010949:Plasma / Q000737:chemistry; D012385:Ronidazole / Q000031:analogs & derivatives / Q000032:analysis* / Q000097:blood / Q000737:chemistry; D013552:Swine; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013997:Time Factors
chemical_list: D008795:Metronidazole; D012385:Ronidazole; D004131:Dimetridazole