Miranda Tiago A, Silva Pedro H R, Pianetti Gerson A, César Isabela C
Departamento de Produtos Farmacêuticos, Faculdade de Farmácia, Universidade Federal de Minas Gerais, Av Pres Antônio Carlos 6627, Belo Horizonte, 31270-901, MG, Brazil.
Malar J. 2015 Jan 28;14:29. doi: 10.1186/s12936-015-0570-1.
Chloroquine and primaquine are the first-line treatment recommended by World Health Organization for malaria caused by Plasmodium vivax. Since the problem of counterfeit or substandard anti-malarials is well established all over the world, the development of rapid and reliable methods for quality control analysis of these drugs is essential. Thus, the aim of this study was to develop and validate a novel UPLC-DAD method for simultaneously quantifying chloroquine and primaquine in tablet formulations.
The UPLC separation was carried out using a Hypersil C18 column (50 × 2.1 mm id; 1.9 μm particle size) and a mobile phase composed of acetonitrile (A) and 0.1% aqueous triethylamine, pH 3.0 adjusted with phosphoric acid (B), at a flow rate 0.6 mL/min. Gradient elution was employed. UV detection was performed at 260 nm. UPLC method was fully validated and the results were compared to a conventional HPLC-DAD method for the analysis of chloroquine and primaquine in tablet formulations.
UPLC method was shown to be linear (r2 > 0.99), precise (CV < 2.0%), accurate (recovery rates from 98.11 to 99.83%), specific, and robust. No significant differences were observed between the chloroquine and primaquine contents obtained by UPLC and HPLC methods. However, UPLC method promoted faster analyses, better chromatographic performance and lower solvent consumption.
The developed UPLC method was shown to be a rapid and suitable technique to quantify chloroquine and primaquine in pharmaceutical preparations and may be successfully employed for quality control analysis.
氯喹和伯氨喹是世界卫生组织推荐的用于治疗间日疟原虫引起的疟疾的一线药物。鉴于假冒或不合格抗疟药的问题在全球普遍存在，开发快速可靠的这些药物质量控制分析方法至关重要。因此，本研究的目的是开发并验证一种用于同时定量片剂制剂中氯喹和伯氨喹的新型超高效液相色谱-二极管阵列检测法（UPLC-DAD法）。
使用Hypersil C18柱（内径50×2.1 mm；粒径1.9μm）进行超高效液相色谱分离，流动相由乙腈（A）和用磷酸调节pH值至3.0的0.1%三乙胺水溶液（B）组成，流速为0.6 mL/min。采用梯度洗脱。在260 nm处进行紫外检测。对超高效液相色谱法进行了全面验证，并将结果与用于分析片剂制剂中氯喹和伯氨喹的传统高效液相色谱-二极管阵列检测法（HPLC-DAD法）进行比较。
超高效液相色谱法显示具有线性（r2＞0.99）、精密度高（CV＜2.0%）、准确度高（回收率为98.11%至99.83%）、专属性强且耐用的特点。超高效液相色谱法和高效液相色谱法测得的氯喹和伯氨喹含量之间未观察到显著差异。然而，超高效液相色谱法分析速度更快、色谱性能更好且溶剂消耗更低。
所开发的超高效液相色谱法是一种快速且适用的技术，可用于定量药物制剂中的氯喹和伯氨喹，并可成功用于质量控制分析。
