Istituto Zooprofilattico Sperimentale del Mezzogiorno, Dipartimento di Chimica, Via Salute, 2, 80055 Portici, NA, Italy.
J Chromatogr A. 2010 Apr 23;1217(17):2832-9. doi: 10.1016/j.chroma.2010.02.047. Epub 2010 Feb 25.
HPLC with fluorescence detection is considered for confirmatory analysis of group B veterinary drugs by the European Union legislation. A procedure for confirming the presence of anti-inflammatory non-steroidal drug (NSAID) residues in bovine milk by reversed phase high-performance liquid chromatography with fluorescence detection is herein described. The native fluorescence of nine drugs belonging to different NSAID sub-classes, namely flurbiprofen, carprofen, naproxen, vedaprofen, 5-hydroxy-flunixin, niflumic acid, mefenamic acid, meclofenamic acid and tolfenamic acid, allowed for detection in bovine milk down to 0.25-20.0 microg/kg. Confirmation of the nine NSAIDs is attained by fluorescence detection at characteristic excitation and emission wavelengths. The procedure described is simple and selective. Limits of quantification (LOQs) ranging between 0.25 and 20 microg/kg were measured; satisfactory trueness and within-laboratory reproducibility data were calculated at LOQ spiking levels, apart from 5-hydroxy-flunixin. The procedure developed is used in our laboratory for confirmation of each one of the above mentioned NSAIDs in bovine milk, to support results after HPLC quantitative analysis with UV-vis detection.
HPLC 与荧光检测被认为是用于欧盟法规中 B 族兽药确证分析的方法。本文描述了一种通过反相高效液相色谱法和荧光检测来确证牛牛奶中抗炎非甾体药物（NSAID）残留的方法。属于不同 NSAID 亚类的九种药物（氟比洛芬、卡洛芬、萘普生、戊地昔布、5-羟基-氟尼辛、尼氟灭酸、甲芬那酸、甲氯芬那酸和托芬那酸）的固有荧光允许在牛牛奶中检测到低至 0.25-20.0 μg/kg 的浓度。通过在特征激发和发射波长处的荧光检测来确认这九种 NSAIDs。所描述的方法简单且具有选择性。除了 5-羟基-氟尼辛之外，在 LOQ 加标水平下计算了 0.25-20 μg/kg 范围内的定量限（LOQs），并得出了令人满意的准确度和实验室内部重现性数据。本实验室使用所开发的方法来确证牛牛奶中的每一种上述 NSAIDs，以支持使用紫外可见检测的 HPLC 定量分析后的结果。
