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流动注射分光光度法通过与铝(III)络合测定药物制剂中的四环素。

Flow injection spectrophotometric determination of tetracycline in a pharmaceutical preparation by complexation with aluminium(III).

作者信息

Liawruangrath Saisunee, Liawruangrath Boonsom, Watanesk Surasak, Ruengsitagoon Wirat

机构信息

Department of Chemistry, Faculty of Science, Chiang Mai University, 50200, Chiang Mai, Thailand.

出版信息

Anal Sci. 2006 Jan;22(1):15-9. doi: 10.2116/analsci.22.15.

Abstract

A rapid flow injection (FI) spectrophotometric procedure for tetracycline determination is described. It is based on the injection of a 100 microl sample solution containing tetracycline into merged streams of aluminium(III) chloride (0.01 mol 1(-1)) and Tris-buffer in the presence of KCl (0.06 mol l(-1)), pH 7.0, with the same optimum flow rate of 3.2 ml min(-1). A yellow Al(III)-tetracycline complex was monitored at 376 nm. The flow injection system and the experimental conditions were optimized by means of the univariate method. The procedure was applied to the determination of tetracycline in pharmaceutical preparations with a high sampling rate of at least 165 h(-1). A high precision with a relative standard deviation was obtained less than 0.72 and 0.30% of 5.0 and 10 microg ml(-1) (n=11), respectively. The detection limit (3sigma) and the quantification limit (10sigma) were 0.07 and 0.72 mg l(-1), respectively. There were no interference effects from traditional excipients in the dosage forms when the method was applied to pharmaceutical preparations. The matrix effect could be reduced by the standard addition method.

摘要

描述了一种用于四环素测定的快速流动注射(FI)分光光度法。该方法基于将含有四环素的100微升样品溶液注入在氯化钾(0.06摩尔/升)存在下、pH 7.0的氯化铝(III)(0.01摩尔/升)和Tris缓冲液的合并流中,最佳流速均为3.2毫升/分钟。在376纳米处监测黄色的铝(III)-四环素络合物。通过单变量法对流动注射系统和实验条件进行了优化。该方法应用于药物制剂中四环素的测定,采样率高达至少165次/小时。对于5.0和10微克/毫升(n = 11),相对标准偏差分别小于0.72%和0.30%,获得了高精度。检测限(3σ)和定量限(10σ)分别为0.07和0.72毫克/升。当该方法应用于药物制剂时,剂型中的传统辅料没有干扰作用。基体效应可通过标准加入法降低。

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