重铬酸钾比色法测定散装和片剂齐多夫定的含量

U. Ogbeide, H. A. Okeri, C. Eboka
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引用次数: 0

摘要

建立了用重铬酸钾在硫酸中氧化齐多夫定(ZDV)的比色法测定原料药和片剂的含量。测定了氧化产物的最大吸收波长(λ max),优化了硫酸、重铬酸钾的浓度和加热时间。在λ max处建立了Beers图,并将其用于纯药物样品的回收率研究。采用酸萃取和甲醇萃取两种方法从片剂样品中提取ZDV。然后用所建立的方法测定该药物在片剂中的百分含量。采用国际人用药品注册技术要求协调委员会(ICH)指南对该方法进行了验证。氧化产物的λ max为602 nm。优化条件为:0.083M(重铬酸钾),12 M(硫酸),90℃加热30 min。Beer’s plot的回归方程为:ZDV的A = 0.4313C + 0.0018 (r2 =0.9995)。标准溶液中ZDV的回收率为100.36%±0.36。因此,所开发的方法是准确和精确的。ZDV不同品牌的含量分别为99.07%±0.83、98.70%±0.76、93.46%±0.72。这些值与用另一种测定方法得到的结果比较良好。这些值在英国药典(90-110%)的规定范围内。检测限和定量限分别为0.004和0.014 mg/ml。所开发的方法简单、准确,利用现成的化学品和设备,而且价格低廉。该方法可用于ZDV的常规测定。关键词:齐多夫定,氧化,比色,吸光度
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Colorimetric determination of zidovudine in bulk and tablet dosage forms using potassium dichromate
A colorimetric method involving the oxidation of zidovudine (ZDV) using potassium dichromate in sulphuric acid has been developed for the determination of ZDV in bulk and tablet dosage forms. The wavelength of maximum absorption (λ max ) of the oxidation product was determined and concentrations of sulphuric acid, potassium dichromate and amount/duration of heat were optimized. Beers plot was constructed at the λ max and used in the recovery studies for pure drug sample. Two methods (acid and methanol extraction) were used to extract ZDV from tablet samples. The developed method was then used to determine the percentage content of the drug in the tablets. The method was validated using the International Council for Harmonization of Technical Requirement for registration of Pharmaceuticals for Human Use (ICH) guideline. The λ max of the oxidation product was found to be 602 nm. The optimized conditions were as follows: 0.083M (potassium dichromate), 12 M (sulphuric acid) and heating at 90oC for 30 mins. The regression equation for the Beer’s plots is: A = 0.4313C + 0.0018 (R 2 =0.9995) for ZDV. The recovery of ZDV from standard solutions was 100.36%±0.36. Thus the developed method was accurate and precise. The percentage contents determined for different brands of ZDV tablets were 99.07%±0.83, 98.70%±0.76, 93.46%±0.72 for the three brands of ZDV. These values compared well with results obtained with use of another method of assay. These values are within the specifications of the British Pharmacopoeia (90-110%). The limits of detection and limits of quantification were 0.004 and 0.014 mg/ml respectively. The developed method is simple, accurate, and utilizes readily available chemicals and equipment, and is inexpensive. It could therefore be used for the routine determination of ZDV. Keywords: Zidovudine, Oxidation, Colorimetric, Absorbance
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