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高效液相色谱法结合光致荧光(PIF)检测和多发射扫描测定依诺沙星、环丙沙星、诺氟沙星和氧氟沙星:应用于尿液和血清

HPLC determination of enoxacin, ciprofloxacin, norfloxacin and ofloxacin with photoinduced fluorimetric (PIF) detection and multiemission scanning: application to urine and serum.

作者信息

Espinosa-Mansilla A, Peña A Muñoz de la, Gómez D González, Salinas F

机构信息

Department of Analytical Chemistry, Faculty of Sciences, University of Extremadura, Campus Universitario, Avda. Elvas S/N Badajoz, 6071 Badajoz, Spain.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Aug 5;822(1-2):185-93. doi: 10.1016/j.jchromb.2005.05.045.

Abstract

The fluorescence emission of the fluoroquinolones enoxacin (ENO), ciprofloxacin (CIPRO), norfloxacin (NOR) and ofloxacin (OFLO) notably increased by UV irradiation during few minutes, in ethanolic-water medium. An HPLC method has been developed, for the determination of these fluoroquinolones, based in the separation of the formed irradiation photoproducts. Optimization of the analytical wavelengths has been carried out by fast multiemission scanning fluorescence detection. The highest sensitivity has been found when measuring at emission wavelengths of 407 and 490 nm, for ENO and OFLO, respectively, and at 444 nm for both NOR and CIPRO (exciting at 277 nm). According to the criterium of Clayton, using 0.05 as false positive and false negative error assurance probabilities, detection limits of 7.3, 6.0, 6.3 and 14.5 ng/mL, for ENO, NOR, CIPRO and OFLO, respectively, have been found. Urine and serum samples have been successfully analyzed, with recovery values ranging among 99-97% and 98-103%, for urine and serum, respectively.

摘要

在乙醇 - 水介质中,紫外照射几分钟后,氟喹诺酮类药物依诺沙星(ENO)、环丙沙星(CIPRO)、诺氟沙星(NOR)和氧氟沙星(OFLO)的荧光发射显著增强。基于对形成的辐照光产物的分离,开发了一种用于测定这些氟喹诺酮类药物的高效液相色谱法。通过快速多发射扫描荧光检测对分析波长进行了优化。分别在407 nm和490 nm的发射波长下测定ENO和OFLO时,以及在444 nm下测定NOR和CIPRO(在277 nm激发)时,发现灵敏度最高。根据克莱顿标准,以0.05作为假阳性和假阴性错误保证概率,分别得出ENO、NOR、CIPRO和OFLO的检测限为7.3、6.0、6.3和14.5 ng/mL。已成功分析了尿液和血清样本,尿液和血清的回收率分别在99 - 97%和98 - 103%之间。

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