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利用金属螯合作用通过荧光分光光度法测定某些喹诺酮类抗菌药物

Spectrofluorometric determination of certain quinolone antibacterials using metal chelation.

作者信息

El-Kommos Michael E, Saleh Gamal A, El-Gizawi Samia M, Abou-Elwafa Mohamed A

机构信息

Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut, Egypt.

出版信息

Talanta. 2003 Jul 27;60(5):1033-50. doi: 10.1016/S0039-9140(03)00171-1.

Abstract

Simple, rapid, reliable, and sensitive spectrofluorometric methods were developed for the determination of eight quinolone antibacterials namely ciprofloxacin, norfloxacin, lomefloxacin, difloxacin, amifloxacin, pefloxacin, ofloxacin, and nalidixic acid. The methods depend on the chelation of each of the studied drugs with zirconium, molybdenum, vanadium or tungsten to produce fluorescent chelates. Different factors affecting the relative fluorescence intensity of the resulting chelates were studied and optimised. At the optimum reaction conditions, the drug-metal chelates showed excitation maxima ranging from 274 to 295 nm and emission maxima ranging from 409 to 495 nm. The chelates were found to be stable at room temperature for 2 days and show good stability upon increasing temperature to 50 degrees C for about 1 h. Rectilinear calibration graphs were obtained in the range of 10-60 ng ml(-1) for each of the investigated drugs and the limits of detection and quantitation ranged from 1.214 to 2.046 and from 4.047 to 6.819 ng ml(-1), respectively. The molar ratios of the formed chelates were determined by Job's method and their association constants were also calculated. The developed methods were applied successfully for the determination of the studied drugs in their pharmaceutical dosage forms with a good precision and accuracy compared to official and reported methods as revealed by t- and F-tests. They were also applied for the determination of studied drugs in spiked urine and plasma samples.

摘要

开发了简单、快速、可靠且灵敏的荧光分光光度法,用于测定8种喹诺酮类抗菌药物,即环丙沙星、诺氟沙星、洛美沙星、二氟沙星、阿米氟沙星、培氟沙星、氧氟沙星和萘啶酸。这些方法基于所研究的每种药物与锆、钼、钒或钨螯合以生成荧光螯合物。研究并优化了影响所得螯合物相对荧光强度的不同因素。在最佳反应条件下,药物 - 金属螯合物的激发最大值在274至295nm范围内,发射最大值在409至495nm范围内。发现螯合物在室温下稳定2天,在温度升至50℃约1小时时也表现出良好的稳定性。对于每种被研究的药物,在10 - 60 ng ml⁻¹范围内获得线性校准曲线,检测限和定量限分别为1.214至2.046 ng ml⁻¹和4.047至6.819 ng ml⁻¹。通过乔布法测定形成的螯合物的摩尔比,并计算它们的缔合常数。与官方和报道的方法相比,通过t检验和F检验表明,所开发的方法成功应用于药物剂型中所研究药物的测定,具有良好的精密度和准确度。它们还应用于加标尿液和血浆样品中所研究药物的测定。

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