Department of Pharmacology and Toxicology, National Veterinary Research Institute, Puławy, Poland.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2013;30(6):977-82. doi: 10.1080/19440049.2013.787652. Epub 2013 May 22.
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.
美他唑仑是一种吡唑酮类非甾体抗炎药，允许在食用动物中使用。根据理事会指令 96/23，由于对消费者健康的潜在风险，必须监测这种药物的残留。美他唑仑被水解为其标记残留 4-甲基氨基安替比林。该化合物进一步代谢为三种主要代谢物：4-甲酰氨基安替比林、4-氨基安替比林和 4-乙酰氨基安替比林。动物组织中 4-甲基氨基安替比林的 MRL 为 100μg/kg。考虑到上述几点，开发了一种用于检测牛肌肉中四种美他唑仑代谢物的方法。分析物通过乙腈和乙酸钠缓冲液的混合物从肌肉中提取。离心后，上清液通过氧化铝小柱，用流动相稀释，并用 LC-MS/MS 分析。四种美他唑仑代谢物在 C8 柱上在 23 分钟内分离，采用甲醇：乙腈：甲酸铵溶液的梯度，并通过正离子化进行分析。方法验证表明，实验室内部重复性在 7-30%之间，回收率在 45-95%之间。该方法符合确证方法的标准，并且由于其劳动效率高，也可用于筛选目的。
