目的 建立基于核磁共振氢谱(1H-NMR)准确定量胶囊中盐酸氨基葡萄糖的方法。方法 1H-NMR测定条件为:脉冲程序zgpr，氢谱宽度6 009 Hz，脉冲宽度11.95 μs，延迟时间6.50 μs，采样温度27 ℃，采样次数32次。结果 以盐酸氨基葡萄糖中δ 3.05的峰作为定量峰，3-(三甲基硅基)氘代丙酸钠(TSP) δ 0的峰作为内标峰，1H-NMR测定盐酸氨基葡萄糖在2.0~12.0 mg·mL-1内具良好的线性关系;盐酸氨基葡萄糖胶囊的平均加样回收率及其RSD分别为103.59%和1.09%(n=9)。结论 1H-NMR具有操作简便、灵敏度高、重现性好、分析时间短等优点，可用于盐酸氨基葡萄糖胶囊制剂的含量测定。
Abstract
OBJECTIVE To establish a 1H-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 1H-NMR analysis, the optimal determination conditions were selected as followsthe pulse sequence was zgpr, hydrogen spectral width was 6 009 Hz, pulse width was 11.95 μs, delay time was 6.50 μs, 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 7X+0.149 9(r=0.999 8) 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.
关键词
核磁共振氢谱 /
盐酸氨基葡萄糖 /
3-(三甲基硅基)氘代丙酸钠 /
内标法 /
含量测定
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Key words
1H-NMR /
glucosamine hydrochloride /
sodium 3-(trimethylsilyl) propionate;internal standard method /
content determination
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中图分类号：
R917
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参考文献
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脚注
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基金
国家自然科学基金资助项目(51173057)
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