Determination of glucosamine hydrochloride in capsules by 1H-NMR method / 中国药学杂志

ABSTRACT

OBJECTIVE: To establish a1 H-NMR internal standard method for measurement of glucosamine hydrochloride in glucosamine hydrochloride capsules. METHODS: For the HPLC-UV method, a China national drug tentative standard (No. YBH11442006) was employed. For the H-NMR analysis, the optimal determination conditions were selected as follows; the pulse sequence was zgpr, hydrogen spectral width was 6 009 Hz, pulse width was 11. 95μs, delay time was 6.50μs, the temperature was 27℃ and the number of scans was 32. RESULTS: The peak of δ 3.05 ppm of the glucosamine hydrochloride and the peak of δ 0 ppm of TSP were selected as quantitative peak and internal standard peak, respectively, and the concentration of the internal standard TSP was 1.02 mmol·L-1. A good linear relationship was obtained with a regression equation as Y = 2.717 IX +0.149 9(r =0.9998) in the concentration range of 2.0-12.0 mg·mL-1. The average recovery rate and the RSD of glucosamine hydrochloride capsules were 103.59% and 1.09% (n = 9), respectively. CONCLUSION: With simple pretreatment, high sensitivity, good repeatability and short analysis time, the NMR-based method could be applied to the measurement of glucosamine hydrochloride in glucosamine hydrochloride capsules.