Multi-residue screening method for the determination of non-steroidal anti-inflammatory drug residues in cow’s milk with HPLC-UV and its application to meloxicam residue depletion study
Multi-residue screening method for the determination of non-steroidal anti-inflammatory drug residues in cow’s milk with HPLC-UV and its application to meloxicam residue depletion study
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发表时间：
2009
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通讯作者：
P. Jedziniak;T. Szprengier-Juszkiewicz;M. Olejnik
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作者：
P. Jedziniak;T. Szprengier-Juszkiewicz;M. Olejnik
建立了一种简便、快速的HPLC-UV法测定牛奶中卡洛芬、双氯芬酸、氟尼辛、美洛昔康、保泰松、托芬那酸、维达洛芬等7种非甾体抗炎药及其代谢产物4-甲氨基安替比林、5-羟基氟尼辛、羟保泰松的残留量。样品制备基于在氯化钠存在下用乙腈进行液-液萃取。在C18柱上用乙腈和乙酸铵缓冲液pH 5.0的梯度进行分析物的分离。紫外检测器波长被编程以提高灵敏度。根据CD/2002/657标准对该方法进行了验证。对于大多数分析物，观察到相对较高的回收率（76%-98%）。实验室内重现性水平在3.6%-17.8%（CV，%）范围内。保泰松、羟保泰松和4-甲氨基安替比林的回收率较低（44%~ 68%），重现性高达41.9%，这可能是由于分析物的不稳定性所致。成功研究了该方法对不同脂肪含量的耐用性。该方法通过用于测定美洛昔康给药奶牛乳汁样品中的美洛昔康残留进行了验证。所获得的结果证实了所开发的方法用于分析牛奶中的NSAID残留物的实用性。
A simple and short HPLC-UV screening method for the determination of residues for seven NSAIDs (carprofen, diclofenac, flunixin, meloxicam, phenylbutazone, tolfenamic acid, vedaprofen) and their three metabolites (4-methylaminoantipyrine, 5-hydroxyflunixin, oxyphenbutazone) in cow’s milk has been developed. The sample preparation was based on liquid-liquid extraction with acetonitrile in the presence of sodium chloride. The separation of analytes was performed on a C18 column with a gradient of acetonitrile and the ammonium acetate buffer pH 5.0. UV-detector wavelength was programmed in order to improve sensitivity. The method was validated according to the CD/2002/657 criteria. For most analytes, relatively high recoveries were observed (76%-98%). Within-laboratory reproducibility levels were in the range of 3.6%-17.8% (CV, %). For phenylbutazone, oxyphenbutazone, and 4-methylaminoantipyrine recoveries were considerably lower (44%-68%) and reproducibility was up to 41.9%, which was probably caused by the instability of analytes. The robustness of the method for different fat content was successfully investigated. The method was verified by its use in the determination of meloxicam residues in milk samples obtained from meloxicam-treated cows. The obtained results confirm the usefulness of the developed method for the analysis of NSAIDs residues in milk.