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化学计量学优化 FIA 法测定奋乃静含量。

Chemometrical optimization FIA of perphenazine assay.

机构信息

School of Chemistry, Cottingham Road, The University of Hull, Hull HU6 7RX, UK.

出版信息

Talanta. 1998 Aug;46(5):897-906. doi: 10.1016/s0039-9140(97)00377-9.

Abstract

A flow injection method for the assay of perphenazine using cerium(IV) as oxidant in a sulphuric acid media was adopted. Different chemometric techniques, considered the main objective of this work, were utilised to optimise sensitivity and sample throughput as a function of five experimental variables. The optimum conditions obtained by the super modified simplex method were, 0.170 M sulphuric acid, 2.13 mM cerium(IV), 2.56 ml min(-1) flow rate, 52 cm coil length, and 136 mul sample loop size. A central composite design was successfully employed, characterising the relation between these variables and the response surface, and hence validating the optimum conditions obtained by the simplex method. Regression analysis of the data from the experimental design, demonstration that a second order polynomial model is an adequate description of the surface over the factor limits studied. Further analysis of the response surface revealed the presence of a broad maximum around the simplex method optimum. A linear calibration curve in the range 50-500 ppm together with a sampling frequency of at least 120 s h(-1) and a relative standard deviation of less than 0.8% were obtained for the determination of perphenazine in its pure analytical grade. Results of the perphenazine assay in pharmaceutical preparations indicates that the method does not suffer interference from excipients rendering the method suitable for the assay of perphenazine in drug formulations.

摘要

采用硫酸介质中以四价铈为氧化剂的流动注射法测定奋乃静。不同的化学计量学技术被认为是这项工作的主要目标,用于优化灵敏度和样品通量作为五个实验变量的函数。通过超改进单纯形法获得的最佳条件为:0.170 M 硫酸、2.13 mM 四价铈、2.56 ml min(-1)流速、52 cm 盘管长度和 136 mul 样品环尺寸。成功地采用了中心复合设计,描述了这些变量与响应面之间的关系,从而验证了单纯形法获得的最佳条件。对实验设计数据的回归分析表明,二次多项式模型是对研究因子极限范围内表面的充分描述。对响应面的进一步分析表明,在单纯形法最优值附近存在一个宽最大值。在纯分析级别的奋乃静中,可获得 50-500 ppm 范围内的线性校准曲线,以及至少 120 s h(-1)的采样频率和小于 0.8%的相对标准偏差。药物制剂中奋乃静测定的结果表明,该方法不受赋形剂的干扰,使该方法适用于药物制剂中奋乃静的测定。

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