The State Laboratory, Backweston Laboratory Complex, Young's Cross, Celbridge, Co. Kildare, Ireland.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2010 Jul;27(7):962-82. doi: 10.1080/19440041003706779.
A sensitive and selective method for the determination of six non-steroidal anti-inflammatory drugs (NSAIDs) in bovine plasma was developed. An improved method for the determination of authorized and non-authorized residues of 10 non-steroidal anti-inflammatory drugs in milk was developed. Analytes were separated and acquired by high performance liquid chromatography coupled with an electrospray ionisation tandem mass spectrometer (ESI-MS/MS). Target compounds were acidified in plasma, and plasma and milk samples were extracted with acetonitrile and both extracts were purified on an improved solid phase extraction procedure utilising Evolute ABN cartridges. The accuracy of the methods for milk and plasma was between 73 and 109%. The precision of the method for authorized and non-authorized NSAIDs in milk and plasma expressed as % RSD, for the within lab reproducibility was less than 16%. The % RSD for authorized NSAIDs at their associated MRL(s) in milk was less than 10% for meloxicam, flunixin and tolfenamic acid and was less than 25% for hydroxy flunixin. The methods were validated according to Commission Decision 2002/657/EC.
建立了一种灵敏、选择性好的测定牛血浆中 6 种非甾体抗炎药(NSAIDs)的方法。建立了一种改进的测定牛奶中 10 种非甾体抗炎药授权和未授权残留的方法。采用高效液相色谱-电喷雾串联质谱(ESI-MS/MS)进行分析和检测。目标化合物在血浆中酸化,血浆和牛奶样品用乙腈提取,两种提取物均用 Evolute ABN 小柱进行改良固相萃取程序纯化。牛奶和血浆中方法的准确度在 73%至 109%之间。牛奶和血浆中授权和未授权 NSAIDs 的方法精密度表示为 % RSD,实验室内重复性小于 16%。牛奶中与相关 MRL(s)相关的授权 NSAIDs 的 % RSD 对于美洛昔康、氟尼辛和托芬那酸小于 10%,对于羟基氟尼辛小于 25%。该方法按照委员会 2002/657/EC 号决定进行了验证。