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根据欧盟第2002/657/EC号决定,开发一种用于测定牛肝和猪肾中十种喹诺酮类药物的高效液相色谱多残留方法。

Development of an HPLC multi-residue method for the determination of ten quinolones in bovine liver and porcine kidney according to the European Union Decision 2002/657/EC.

作者信息

Christodoulou Eleni A, Samanidou Victoria F, Papadoyannis Ioannis N

机构信息

Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece.

出版信息

J Sep Sci. 2008 Jan;31(1):119-27. doi: 10.1002/jssc.200700297.

DOI:10.1002/jssc.200700297
PMID:18081209
Abstract

A sensitive multi-residue analytical method was developed for the determination of ten quinolones: enoxacin, ofloxacin, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, oxolinic acid, nalidixic acid, and flumequine in bovine liver and porcine kidney. A simple liquid extraction step followed by a solid phase extraction clean up procedure was applied for the extraction of quinolones from liver and kidney tissues. Recoveries of the extraction varied between 82 and 88% for bovine liver and 92 and 95% for porcine kidney. Separation was performed on an ODS-3 PerfectSil Target (250 x 4 mm) 5 microm analytical column at 25 degrees C. The mobile phase consisted of a mixture of TFA 0.1%-CH(3)CN-CH(3)OH, delivered at a flow rate of 1.2 mL/min according to a gradient program. Elution of quinolones and the internal standard (caffeine, 7.5 ng/microL) was complete within 27 min. Photodiode array detection was used for monitoring the eluants at 275 and 255 nm. The method was fully validated according to the European Union Decision 2002/657/EC, determining linearity, selectivity, decision limit, detection capability, accuracy, and precision. The LODs of the specific method of quinolone determination in bovine liver varied between 3 and 7 microg/kg and in porcine kidney between 3 and 4 microg/kg.

摘要

开发了一种灵敏的多残留分析方法,用于测定牛肝和猪肾中的十种喹诺酮类药物:依诺沙星、氧氟沙星、诺氟沙星、环丙沙星、达氟沙星、恩诺沙星、沙拉沙星、恶喹酸、萘啶酸和氟甲喹。采用简单的液液萃取步骤,随后进行固相萃取净化程序,从肝脏和肾脏组织中提取喹诺酮类药物。牛肝的萃取回收率在82%至88%之间,猪肾的萃取回收率在92%至95%之间。在25℃下,于ODS-3 PerfectSil Target(250×4mm)5μm分析柱上进行分离。流动相由0.1%三氟乙酸-乙腈-甲醇的混合物组成,按照梯度程序以1.2mL/min的流速输送。喹诺酮类药物和内标(咖啡因,7.5ng/μL)在27分钟内洗脱完全。使用光电二极管阵列检测在275nm和255nm处监测洗脱液。该方法根据欧盟第2002/657/EC号决定进行了全面验证,测定了线性、选择性、决策限、检测能力、准确度和精密度。牛肝中喹诺酮类药物特定测定方法的检测限在3至7μg/kg之间,猪肾中的检测限在3至4μg/kg之间。

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