一种用于测定药物样品中姜黄素并进行稳定性研究的简单、灵敏且快速的等度反相高效液相色谱法。

A simple, sensitive and rapid isocratic reversed-phase high-performance liquid chromatography method for determination and stability study of curcumin in pharmaceutical samples.

作者信息

Amanolahi Farjad, Mohammadi Ali, Kazemi Oskuee Reza, Nassirli Hooriyeh, Malaekeh-Nikouei Bizhan

机构信息

Department of Drug and Food Control, School of Pharmacy, Tehran University of Medical Science, Tehran, Iran.

Department of Medical Biotechnology, School of Medicine, Mashhad University of Medical Sciences, Mashhad, Iran.

出版信息

Avicenna J Phytomed. 2017 Sep-Oct;7(5):444-453.

PMID:29062806

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC5641419/

Abstract

OBJECTIVE

This study was designed to develop and validate a new reversed-phase high-performance liquid chromatography (RP-HPLC) method based on Q (R) International Conference on Harmonization (ICH) guideline for determination of curcumin in pharmaceutical samples.

MATERIALS AND METHODS

The HPLC instrument method was optimized with isocratic elution with acetonitrile: ammonium acetate (45:55, v/v, pH 3.5), C18 column (150 mm×4.6 mm×5 µm particle size) and a flow rate of 1 ml/min in ambient condition and total retention time of 17 min. The volume of injection was set at 20 µl and detection was recorded at 425 nm. The robustness of the method was examined by changing the mobile phase composition, mobile phase pH, and flow rate.

RESULTS

The method was validated with respect to precision, accuracy and linearity in a concentration range of 2-100 µg/ml. The limit of detection (LOD) and limit of quantification (LOQ) were 0.25 and 0.5 µg/ml, respectively. The percentage of recovery was 98.9 to 100.5 with relative standard deviation (RSD) < 0.638%.

CONCLUSION

The method was found to be simple, sensitive and rapid for determination of curcumin in pharmaceutical samples and had enough sensitivity to detect degradation product of curcumin produced under photolysis and hydrolysis stress condition.

摘要

目的

本研究旨在根据国际协调会议（ICH）指南开发并验证一种新的反相高效液相色谱（RP-HPLC）方法，用于测定药物样品中的姜黄素。

材料与方法

采用乙腈：醋酸铵（45:55，v/v，pH 3.5）等度洗脱，C18柱（150 mm×4.6 mm×5 µm粒径），在环境条件下流速为1 ml/min，总保留时间为17 min，对HPLC仪器方法进行优化。进样体积设定为20 µl，检测波长为425 nm。通过改变流动相组成、流动相pH值和流速来考察该方法的稳健性。