Rapid method for the determination of metamizole residues in bovine muscle by LC-MS/MS. 2013

Piotr Jedziniak, and Konrad Pietruk, and Edyta Śledzińska, and Małgorzata Olejnik, and Teresa Szprengier-Juszkiewicz, and Jan Żmudzki
Department of Pharmacology and Toxicology, National Veterinary Research Institute, Puławy, Poland. jedzi@piwet.pulawy.pl

Metamizole is a pyrazolone non-steroidal anti-inflammatory drug allowed for use in food-producing animals. According to Council Directive 96/23, residues of this drug have to be monitored because of the potential risk to consumers' health. Metamizole is hydrolysed to its marker residue 4-methylaminoantypyrine.This compound is further metabolised to three main metabolites: 4-formylaminoantipyrine, 4-aminoantipyrine and 4-acetylaminoantipyrine. The MRL of 4-methylaminoantipyrine in animal tissues is 100 µg kg(-1). Considering the above points, a method for the detection of four metamizole metabolites in bovine muscles was developed. Analytes were extracted from muscle by a mixture of acetonitrile and sodium acetate buffer. After centrifugation, the supernatant was passed through alumina cartridges, diluted with mobile phase and analysed by using LC-MS/MS. Four metamizole metabolites were separated on a C8 column in 23 min with a gradient of methanol:acetonitrile:ammonium formate solution and analysed by using positive ionisation. Validation of the method indicated a within-laboratory reproducibility in the range of 7-30% and recovery in the range of 45-95%. The method fulfils the criteria for confirmatory methods and, thanks to its labour efficiency, may also be used for screening purposes.

UI MeSH Term Description Entries
D009132 Muscles Contractile tissue that produces movement in animals. Muscle Tissue,Muscle,Muscle Tissues,Tissue, Muscle,Tissues, Muscle
D002417 Cattle Domesticated bovine animals of the genus Bos, usually kept on a farm or ranch and used for the production of meat or dairy products or for heavy labor. Beef Cow,Bos grunniens,Bos indicus,Bos indicus Cattle,Bos taurus,Cow,Cow, Domestic,Dairy Cow,Holstein Cow,Indicine Cattle,Taurine Cattle,Taurus Cattle,Yak,Zebu,Beef Cows,Bos indicus Cattles,Cattle, Bos indicus,Cattle, Indicine,Cattle, Taurine,Cattle, Taurus,Cattles, Bos indicus,Cattles, Indicine,Cattles, Taurine,Cattles, Taurus,Cow, Beef,Cow, Dairy,Cow, Holstein,Cows,Dairy Cows,Domestic Cow,Domestic Cows,Indicine Cattles,Taurine Cattles,Taurus Cattles,Yaks,Zebus
D002853 Chromatography, Liquid Chromatographic techniques in which the mobile phase is a liquid. Liquid Chromatography
D004177 Dipyrone A drug that has analgesic, anti-inflammatory, and antipyretic properties. It is the sodium sulfonate of AMINOPYRINE. Metamizole,Methampyrone,Noramidopyrine Methanesulfonate,Algopyrin,Analgin,Biopyrin,Dipyronium,Metamizol,Metamizole Sodium,Methamizole,Narone,Noramidopyrine Methanesulfonate Sodium,Normelubrine,Novalgetol,Novalgin,Novamidazophen,Novaminsulfone,Optalgin,Pyralgin,Sulpyrin,Sulpyrine
D004350 Drug Residues Drugs and their metabolites which are found in the edible tissues and milk of animals after their medication with specific drugs. This term can also apply to drugs found in adipose tissue of humans after drug treatment. Drug Residue,Residue, Drug,Residues, Drug
D000818 Animals Unicellular or multicellular, heterotrophic organisms, that have sensation and the power of voluntary movement. Under the older five kingdom paradigm, Animalia was one of the kingdoms. Under the modern three domain model, Animalia represents one of the many groups in the domain EUKARYOTA. Animal,Metazoa,Animalia
D000894 Anti-Inflammatory Agents, Non-Steroidal Anti-inflammatory agents that are non-steroidal in nature. In addition to anti-inflammatory actions, they have analgesic, antipyretic, and platelet-inhibitory actions. They act by blocking the synthesis of prostaglandins by inhibiting cyclooxygenase, which converts arachidonic acid to cyclic endoperoxides, precursors of prostaglandins. Inhibition of prostaglandin synthesis accounts for their analgesic, antipyretic, and platelet-inhibitory actions; other mechanisms may contribute to their anti-inflammatory effects. Analgesics, Anti-Inflammatory,Aspirin-Like Agent,Aspirin-Like Agents,NSAID,Non-Steroidal Anti-Inflammatory Agent,Non-Steroidal Anti-Inflammatory Agents,Nonsteroidal Anti-Inflammatory Agent,Anti Inflammatory Agents, Nonsteroidal,Antiinflammatory Agents, Non Steroidal,Antiinflammatory Agents, Nonsteroidal,NSAIDs,Nonsteroidal Anti-Inflammatory Agents,Agent, Aspirin-Like,Agent, Non-Steroidal Anti-Inflammatory,Agent, Nonsteroidal Anti-Inflammatory,Anti-Inflammatory Agent, Non-Steroidal,Anti-Inflammatory Agent, Nonsteroidal,Anti-Inflammatory Analgesics,Aspirin Like Agent,Aspirin Like Agents,Non Steroidal Anti Inflammatory Agent,Non Steroidal Anti Inflammatory Agents,Nonsteroidal Anti Inflammatory Agent,Nonsteroidal Anti Inflammatory Agents,Nonsteroidal Antiinflammatory Agents
D053719 Tandem Mass Spectrometry A mass spectrometry technique using two (MS/MS) or more mass analyzers. With two in tandem, the precursor ions are mass-selected by a first mass analyzer, and focused into a collision region where they are then fragmented into product ions which are then characterized by a second mass analyzer. A variety of techniques are used to separate the compounds, ionize them, and introduce them to the first mass analyzer. For example, for in GC-MS/MS, GAS CHROMATOGRAPHY-MASS SPECTROMETRY is involved in separating relatively small compounds by GAS CHROMATOGRAPHY prior to injecting them into an ionization chamber for the mass selection. Mass Spectrometry-Mass Spectrometry,Mass Spectrometry Mass Spectrometry,Mass Spectrometry, Tandem

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