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采用夹管电磁阀和微型泵的多通道流动系统。分光光度法测定药物制剂中的对乙酰氨基酚。

Multicommuted flow system employing pinch solenoid valves and micro-pumps. Spectrophotometric determination of paracetamol in pharmaceutical formulations.

作者信息

Lavorante André F, Pires Cherrine K, Reis Boaventura F

机构信息

Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, PO Box 96, 13400-970 Piracicaba, SP, Brazil.

出版信息

J Pharm Biomed Anal. 2006 Oct 11;42(4):423-9. doi: 10.1016/j.jpba.2006.04.013. Epub 2006 May 26.

Abstract

A multicommuted spectrophotometric flow-based procedure for the determination of paracetamol in pharmaceutical formulations is proposed. The method is based on the reaction of paracetamol with sodium hypochlorite forming N-acetyl-p-benzoquinoneimine, which reacts with sodium salicylate in alkaline medium producing a blue indophenol dye that was measured at 640nm. The flow system was designed employing four pinch solenoid valves and two solenoid micro-pumps, which were assembled aiming to obtain a compact module, resulting in minimization of reagents consumption and waste generation. Aiming to prove the usefulness of flow system an analytical procedure for paracetamol determination in pharmaceutical formulations was developed. To allow accuracy assessment samples were also analyzed using the AOAC reference method. Applying the paired t-test between results no significant difference at the 95% confidence level was observed. Other profitable features such as a linear response ranging from 5.0 to 125.0mgl(-1) (R=0.9992, n=7), a sampling rate of 60 determinations per hour, a detection limit of 0.4mgl(-1) paracetamol, a relative standard deviation of 1.5% (n=11) for a typical sample solution containing 25.0mgl(-1) paracetamol, reagent consumption of 1.28mg sodium hypochlorite and 6.4mg sodium salicylate per determination were also achieved.

摘要

本文提出了一种基于多通道流动注射分光光度法测定药物制剂中对乙酰氨基酚的方法。该方法基于对乙酰氨基酚与次氯酸钠反应生成N-乙酰对苯醌亚胺,后者在碱性介质中与水杨酸钠反应生成蓝色吲哚酚染料,于640nm处进行测定。流动注射系统采用四个夹管电磁阀和两个电磁微型泵进行设计,组装目的是获得一个紧凑的模块,从而最大限度地减少试剂消耗和废物产生。为证明流动注射系统的实用性,开发了一种测定药物制剂中对乙酰氨基酚的分析方法。为评估准确性,还采用美国官方分析化学师协会(AOAC)的参考方法对样品进行了分析。通过对结果进行配对t检验,在95%置信水平下未观察到显著差异。该方法还具有其他优点,如线性响应范围为5.0至125.0mg L-1(R = 0.9992,n = 7),每小时采样率为60次测定,对乙酰氨基酚的检测限为0.4mg L-1,对于含25.0mg L-1对乙酰氨基酚的典型样品溶液,相对标准偏差为1.5%(n = 11),每次测定次氯酸钠试剂消耗量为1.28mg,水杨酸钠试剂消耗量为6.4mg。

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