微波辅助碱性水解分光光度法测定对乙酰氨基酚

Spectrophotometric determination of paracetamol with microwave assisted alkaline hydrolysis.

作者信息

Xu Chunli, Li Baoxin

机构信息

Department of Chemistry, School of Chemistry and Materials Science, Shaanxi Normal University, Xi'an 710062, PR China.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2004 Jul;60(8-9):1861-4. doi: 10.1016/j.saa.2003.10.003.

DOI:10.1016/j.saa.2003.10.003

PMID:15248961

Abstract

A novel and rapid spectrophotometric method for the determination of paracetamol is proposed in this paper. The proposed method is based on the microwave assisted alkaline hydrolysis of paracetamol to p-aminophenol that reacts with S2- in the presence of Fe3+ as oxidant to produce a methylene blue-like dye having an absorptivity maximum at 540 nm. The experiment showed that paracetamol could be hydrolysed quantitatively to p-aminophenol in only 1.5 min under radiation power 640 W using a microwave in NaOH medium. The system obeys Beer's law in the range of 0-3.0 x 10(-4) mol l(-1) paracetamol. The molar absorptivity and Sandell's sensitivity were found to be 3.2 x 10(-3) l mol(-1) cm(-1) and 0.047 microg cm(-2), respectively. The relative standard deviation (n=11) was 1.7% for 8.0 x 10(-5) mol l(-1) paracetamol. The method has been applied successfully to analysis of paracetamol in pharmaceutical preparation.

摘要

本文提出了一种测定扑热息痛的新颖快速分光光度法。该方法基于扑热息痛在微波辅助下于碱性条件下水解为对氨基酚，对氨基酚在Fe³⁺作为氧化剂存在的情况下与S²⁻反应，生成一种在540 nm处有最大吸收的类似亚甲基蓝的染料。实验表明，在640 W辐射功率下，使用微波，在NaOH介质中，扑热息痛仅需1.5分钟就能定量水解为对氨基酚。该体系在0 - 3.0×10⁻⁴ mol·L⁻¹扑热息痛范围内符合比尔定律。摩尔吸光系数和桑德尔灵敏度分别为3.2×10⁻³ L·mol⁻¹·cm⁻¹和0.047 μg·cm⁻²。对于8.0×10⁻⁵ mol·L⁻¹扑热息痛，相对标准偏差（n = 11）为1.7%。该方法已成功应用于药物制剂中扑热息痛的分析。