金丝桃苷对照品的定值研究

目的: 采用质量平衡法测定金丝桃苷对照品的含量,同时采用核磁共振定量法加以佐证. 方法: 采用高效液相色谱法测定样品色谱纯度,同时测定水分、残留溶剂及炽灼残渣,以质量平衡法计算金丝桃苷的含量,并对测定结果的不确定度进行评估;同时,以核磁共振定量法一步测定金丝桃苷含量. 结果: 金丝桃苷高效液相色谱纯度测定均值为98.49%,水分测定均值为2.80%,残留溶剂乙醇测定均值为3.11%,炽灼残渣测定均值为0.19%;以质量平衡法计算其含量为92.5%,扩展不确定度为0.2%;核磁共振定量法测定含量为92.1%. 结论: 质量平衡法与核磁共振定量法测定的金丝桃苷含量结果基本一致,2种方法能够更好地保证金丝桃苷对照品赋值的准确性.

Objective: To determine the content of hyperoside reference substance by the mass balance method and quantitative nuclear magnetic resonance method(qNMR). Methods: The chromatographic purity of the sample was determined by HPLC method,and contents of moisture,residual solvent and ignition residue were all determined.The content of hyperoside was calculated by mass balance method.The uncertainty was also calculated.In addition,qNMR was applied to measure the content of hyperoside. Results: The average tested contents of chromatographic purity,moisture,residual ethanol and ignition residue were 98.49%,2.80%,3.11% and 0.19%,respectively.The content of hyperoside was 92.5% by mass balance method with the extended uncertainty of 0.2%,and was 92.1% by qNMR. Conclusion: The determined content of hyperoside by mass balance method was in accordance with the result by qNMR,and both methods could ensure the accuracy of the certification of hyperoside.

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