熊果苷对照品的定值研究

目的：联合质量平衡法、差示扫描量热法及定量核磁共振法3种定值方法测定熊果苷对照品的纯度。方法：首先，采用高效液相色谱法和气相色谱法测定熊果苷对照品的色谱纯度，采用卡尔费休库伦法、电感耦合等离子体质谱法、顶空气相色谱法分别测定其水分、灰分和残留溶剂，由质量平衡法计算熊果苷对照品的纯度；其次，采用差示扫描量热法对熊果苷对照品纯度加以验证；最后，以定量核磁共振法测定其绝对纯度。结果：质量平衡法和差示扫描量热法定值结果经科克伦法判定互为等精度，取其算术平均值作为最终定值结果，即熊果苷对照品纯度为99.12%，RSD为0.029%；定量核磁共振法测定结果为99.12%，RSD为0.036%。结论：质量平衡法、差示扫描量热法及定量核磁共振法对熊果苷对照品的定值结果基本一致，3种方法能够更好地保证熊果苷对照品赋值的准确性。

Objective:To determine the content of arbutin by the three methods including mass balance,differential scanning calorimetry(DSC)and quantitative nuclear magnetic resonance(qNMR). Methods:Firstly,the chromatographic purity of arbutin reference substance was determined by HPLC & GC methods. Moisture,ignition residue and residual solvents were determined by Karl -Fischer-Coulomb method,inductively coupled with plasma mass spectrometry and headspace gas chromatography,respectively. The purity of arbutin reference substance was calculated by mass balance method. Secondly,the purity of arbutin reference substance was verified by differential scanning calorimetry. Finally,the absolute purity of arbutin reference substance was determined by qNMR. Results:The results of mass balance method and differential scanning calorimetry were of equal precision by Cochran test. Thus,the arithmetic average value was 99.12% with RSD of 0.029%,which was taken as the final content of arbutin reference substance. And the result of qNMR was 99.12% with RSD of 0.036%. Conclusion:The assignment results of mass balance,differential scanning calorimetry and qNMR were consistent,and three methods can guarantee the accuracy of the assignment.

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