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响应面法分光光度法测定尿液和药物制剂中两种β-肾上腺素激动剂-铽化学传感器。

Response Surface Methodology for Spectrophotometric Determination of Two β-Adrenergic Agonists-Terbium Chemosensors in Urine and Pharmaceutical Dosage Forms.

机构信息

Department of Chemistry and Earth Sciences, College of Arts and Sciences, Qatar University, Doha 2713, Qatar.

Pharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo University, Cairo 11562, Egypt.

出版信息

J AOAC Int. 2021 May 21;104(2):355-367. doi: 10.1093/jaoacint/qsaa131.

DOI:10.1093/jaoacint/qsaa131
PMID:33871029
Abstract

BACKGROUND

According to literature reports, none of the previous methods of analysis had touched the multivariate approach for the quantification of significant factors affecting the interaction of dobutamine or hexoprenaline with Terbium.

OBJECTIVE

Two novel β-adrenergic agonists-lanthanide chemosensors were prepared for the determination of dobutamine and hexoprenaline in their pure and pharmaceutical dosage forms and in urine samples. Fabrication of the two chemosensors was based on their ligand-metal interaction with the lanthanide Terbium.

METHODS

A Plackett-Burman Design (PBD) was selected for the screening of four main variables (reaction time, metal volume, pH, and temperature). Applying Response Surface Methodology (RSM), a Central Composite Design (CCD) was executed for the optimization of the significant factors with narrower upper and lower limits. Spectrophotometric technique was exploited for the analysis of the two chemosensors.

RESULTS

Maximum absorption was obtained at 299 and 298 nm for dobutamine-terbium and hexoprenaline-terbium complexes, respectively. Only factors that were found to bear significant effects on the formed complexes were promoted to the optimization level. Model verification was carried out, where target results coincided with those at the predicted levels, indicating the efficiency of the two proposed models. Validation of the proposed was implemented and linear ranges were found to be 3.30-13.50 and 1.90-10.00 µg/mL, for dobutamine and hexoprenaline, respectively.

CONCLUSIONS

Recovery and relative standard deviation values by application in pure powder, pharmaceutical dosage forms and spiked urine samples indicated high accuracy and reproducibility. Wide-ranging linear values and comparatively low detection limits inferred the effectiveness of the proposed method.

HIGHLIGHTS

RSM for optimization of spectrophotometric determination of dobutamine and hexoprenaline β-adrenergic agonists-lanthanide chemosensors; PBD was used for screening and CCD for optimization of variables affecting the spectrophotometric method; Determination of dobutamine and hexoprenaline in pure powder, pharmaceutical dosage form, and spiked urine samples was accomplished after method validation.

摘要

背景

根据文献报道,以前的分析方法都没有涉及到多变量方法来定量分析影响二羟苯丙胺或六羟肾上腺素与铽相互作用的重要因素。

目的

制备了两种新型的β-肾上腺素能激动剂-镧系化学传感器,用于测定其纯品和制剂以及尿液样品中的二羟苯丙胺和六羟肾上腺素。两种化学传感器的制备基于它们与镧系元素铽的配体-金属相互作用。

方法

选择 Plackett-Burman 设计(PBD)筛选四个主要变量(反应时间、金属体积、pH 值和温度)。应用响应面法(RSM),执行中心复合设计(CCD)以优化具有较窄上下限的重要因素。分光光度技术用于分析两种化学传感器。

结果

二羟苯丙胺-铽和六羟肾上腺素-铽配合物的最大吸收分别在 299 和 298nm 处获得。仅促进对形成的配合物有显著影响的因素进入优化水平。进行了模型验证,目标结果与预测水平一致,表明了两个提出的模型的效率。对提出的方法进行了验证,发现二羟苯丙胺和六羟肾上腺素的线性范围分别为 3.30-13.50 和 1.90-10.00μg/mL。

结论

在纯粉、制剂和加标尿液样品中的应用表明回收率和相对标准偏差值具有较高的准确性和重现性。广泛的线性值和相对较低的检测限表明该方法的有效性。

重点

应用 RSM 优化二羟苯丙胺和六羟肾上腺素β-肾上腺素能激动剂-镧系化学传感器的分光光度法测定;PBD 用于筛选,CCD 用于优化影响分光光度法的变量;在方法验证后,完成了纯品、制剂和加标尿液样品中二羟苯丙胺和六羟肾上腺素的测定。

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