NGHIÊN CỨU ĐIỀU CHẾ QUERCETIN DƯỢC DỤNG

Abstract

  Background: Studies on the synthesis of quercetin from rutin have also been conducted in Vietnam; however, there are numerous obstacles in the way of preparing pure quercetin, and the quality of the hydrolyzed products has not been fully evaluated in accordance with pharmaceutical standards. The "Research on the preparation of quercetin for pharmaceutical grade" was undertaken for this reason. Objectives: To develope a process for preparing quercetin from rutin that meets USP44 pharmacopoeia standards and evaluated the quality indicators of quercetin according to the requirements of the pharmacopoeia treatise. Materials and methods: Research subjects: Rutin (extracted from Flos Sophorae, 95%) - Vietnam, chemical solvents that match AR standards. Method: Using basic reactions in organic chemistry to semi-synthesize quercetin from rutin; Monitor reaction progress using thin layer chromatography (TLC); Check product purity by TLC and melting temperature measurement. Evaluate of semi-synthetic quercetin quality by HPLC method; Validate the quercetin quantification method according to ICH guidelines; Determine product structure through spectral analysis methods: mass spectrometry (MS); infrared (IR) spectroscopy and nuclear magnetic resonance spectroscopy (¹H-NMR and ¹³C-NMR). Results: Semi-synthesized quercetin from rutin with a scale of 10.0g/batch, using a mixture of 96% ethanol/20% HCl (ratio 3:1), water bath temperature 80-90ºC, in 2 hours, filtered to collect crude quercetin product. Survey of purification methods: using solvents (isopropanol, ethanol, dichloromethane), changing pH to obtain results: Purifying crude quercetin in two steps, (1): Changing pH gives pH fractionation results 4 for the product with a content of 99.8%, total impurities of 0.3%, meeting the requirements mentioned in the pharmacopoeia monograph; (2): Recrystallize in hot 96% ethanol at a ratio of 1:30. The overall process efficiency is about 47%, quercetin products meet the quality criteria required in the American pharmacopoeia monograph USP44. The quantitative method has been validated according to ICH guidelines. Quercetin structure was confirmed by spectroscopic analysis methods (IR, MS, NMR) and the spectral values were equivalent to references. Conclusions: A process for preparing quercetin has been developed to satisfy quality criteria according to the treatise of the American Pharmacopoeia USP44.