灵敏云点萃取法分光光度法测定制剂中盐酸异苏嘌呤的含量

H. Hadi, Wasan A. Al-Uzri
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引用次数: 0

摘要

提出了一种简便、高灵敏度的浊点萃取法,用于纯品和药用样品中微量盐酸异苏嘌呤(ISX)的富集。ISX与重氮磺胺在碱性介质中重氮偶氮偶联后,将偶氮染料产物定量提取到Triton X-114富相中,溶解于乙醇中,在490 nm处分光光度测定。对建议的反应进行了有萃取和无萃取的研究,并对间歇法和CPE法进行了简单的比较。分析变量包括试剂浓度,Triton X-114和碱,孵育温度和时间仔细研究。在所选择的最佳条件下,批法和CPE法的ISX检出限分别为0.26和0.09µg/mL,校准曲线的线性范围为1 ~ 9和0.5 ~ 8µg/mL。两种方法的相对标准偏差(RSD %)分别为1.98和2.67%,加样回收率分别为100.14%和99.63%。该方法具有较高的准确度和重复性,可成功地用于药物制剂中ISX的常规分析。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Sensitive Cloud Point Extraction Method for the Determination of Isoxsuprine Hydrochloride in Pharmaceutical forms using Spectrophotometry
      A simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected optimum conditions, the linearity ranges of calibration curves were 1-9 and 0.5-8 µg/mL with detection limits of 0.26 and 0.09 µg/mL of ISX for batch and CPE methods respectively. A relative standard deviation (RSD %) best than 1.98 and 2.67 % with the percentage recoveries range 100.14 and 99.63 % were obtained for both methods respectively. The proposed methods were successfully used in routine analysis of ISX in pharmaceutical forms with high accuracy and reproducibility.
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