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奥美拉唑伏安法测定方法开发中的实验设计

Experimental design in the development of voltammetric method for the assay of omeprazole.

作者信息

Pinzauti S, Gratteri P, Furlanetto S, Mura P, Dreassi E, Phan-Tan-Luu R

机构信息

Dipartimento di Scienze Farmaceutiche, Università di Firenze, Italy.

出版信息

J Pharm Biomed Anal. 1996 Jun;14(8-10):881-9. doi: 10.1016/0731-7085(95)01683-x.

DOI:10.1016/0731-7085(95)01683-x
PMID:8817992
Abstract

A multivariate strategy was used to optimize an adsorptive stripping voltammetric method for the determination of the antiulcer drug omeprazole. A 3/4 matrix was used for the variable screening while a central composite design was chosen in the subsequent step to evaluate the response surfaces. Simultaneous optimization of the response peak height (hp) and peak half width w1/2), the latter being a peak shape measure, was achieved. The factors accumulation time, pulse amplitude, scan rate and stirring rate were all found to be statistically significant for the response hp, while for the response w1/2 only the stirring rate was found to be significant. The optimized method shows a good linearity between peak height and analyte concentration in the concentration range from 8.33 x 10(-9) M to 1.42 x 10(-7) M with a LOD of 6.5 x 10(-9) M. The mean recovery of omeprazole in capsules was 101.9% with a SD of 2.04 (RSD = 200).

摘要

采用多变量策略优化了一种用于测定抗溃疡药物奥美拉唑的吸附溶出伏安法。在变量筛选中使用3/4矩阵,随后选择中心复合设计来评估响应面。实现了响应峰高(hp)和峰半高宽(w1/2,后者是峰形指标)的同时优化。发现富集时间、脉冲幅度、扫描速率和搅拌速率对响应hp均具有统计学意义,而对于响应w1/2,仅搅拌速率具有显著意义。优化后的方法在8.33×10⁻⁹ M至1.42×10⁻⁷ M的浓度范围内,峰高与分析物浓度之间呈现良好的线性关系,检测限为6.5×10⁻⁹ M。胶囊中奥美拉唑的平均回收率为101.9%,标准差为2.04(相对标准偏差=2.00)。

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