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基于可取性函数的多目标优化策略用于血浆和制剂中诺氟沙星和替硝唑的微乳液液相色谱分离与定量分析。

Multiobjective optimization strategy based on desirability functions used for the microemulsion liquid chromatographic separation and quantification of norfloxacin and tinidazole in plasma and formulations.

作者信息

Abou-Taleb Noura Hemdan, El-Wasseef Dalia Rashad, El-Sherbiny Dina Tawfik, El-Ashry Saadia Mohamed

机构信息

Medicinal Chemistry Department, Faculty of Pharmacy, Mansoura University, Mansoura, Egypt.

出版信息

J Sep Sci. 2015 Mar;38(6):901-8. doi: 10.1002/jssc.201401203. Epub 2015 Feb 10.

Abstract

The aim of the present study was to optimize a microemulsion liquid chromatography method for the simultaneous determination of norfloxacin and tinidazole binary mixture using a chemometric protocol. Optimization experiments were conducted through a process of screening and optimization. A 2(7-4) fractional factorial design was used as screening design. While the location of optimum conditions was established by applying Derringer's desirability function. The optimal mobile phase composition was predicted to be: 3.5% w/v SDS, 10.03% v/v 1-propanol, 0.5% v/v 1-octanol, and 0.3% triethylamine in 0.02 M phosphoric acid at pH 6.5. The mobile phase was delivered isocratically at a flow rate of 1 mL/min with UV detection at 290 nm. Tinidazole and norfloxacin were eluted with retention times of 1.8 and 5.8 min, respectively. The calibration plots displayed good linear relationships in the concentration ranges of 0.5-50 and 0.75-75 μg/mL for norfloxacin and tinidazole, respectively. The method was successfully applied for determination of both drugs in pharmaceutical dosage forms and real human plasma. Where the accuracy was proved by the low values of % error and high values of recovery, also the relative standard deviation for the results did not exceed 1.5%, proving the precision of the method.

摘要

本研究的目的是采用化学计量学方法优化一种微乳液液相色谱法,用于同时测定诺氟沙星和替硝唑二元混合物。通过筛选和优化过程进行优化实验。采用2(7-4)分式析因设计作为筛选设计。同时,通过应用德林格合意函数确定最佳条件的位置。预测最佳流动相组成为:在pH 6.5的0.02 M磷酸中,3.5% w/v十二烷基硫酸钠、10.03% v/v正丙醇、0.5% v/v正辛醇和0.3%三乙胺。流动相以1 mL/min的流速等度输送,在290 nm处进行紫外检测。替硝唑和诺氟沙星的保留时间分别为1.8和5.8分钟。校准曲线在诺氟沙星和替硝唑的浓度范围分别为0.5-50和0.75-75 μg/mL时显示出良好的线性关系。该方法成功应用于药物剂型和实际人血浆中两种药物的测定。通过低误差百分比值和高回收率值证明了准确性,结果的相对标准偏差也不超过1.5%,证明了该方法的精密度。

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