两种定值方法测定阿司匹林丁香酚酯对照品的含量

Content Determination of Aspirin Eugenol Ester Reference Substance by Two Measuring Methods

目的：采用质量平衡法与核磁共振法,测定阿司匹林丁香酚酯（aspirin eugenol ester,AEE）对照品含量。方法：采用高相液相色谱测定纯度,采用干燥失质量法测定水分和挥发性物质,炽灼残渣测定无机盐杂质,根据质量平衡法计算AEE对照品含量。建立核磁共振定量测定AEE含量的方法,仪器温度25℃,扫描次数（NS）16次,弛豫延迟时间（Dl）15 s。结果：质量平衡法测定的AEE对照品含量为99.82%;核磁共振定值结果为99.55%,AEE和内标物（1,4-二硝基苯）峰面积的比值与质量比在3-21 mg范围内呈良好线性关系（R2=0.999）,日内精密度的RSD值为0.04%（n=5）,重复性的RSD值为0.19%（n=5）,稳定性测定的RSD值为0.57%。结论：2种方法相互验证,测定结果基本一致。

OBJECTIVE： To determine the content of aspirin eugenol ester（ AEE） reference substance by by the mass balance method and the nuclear magnetic resonance（ NMR） method. METHODS： Chromatogram purity was determined by HPLC,the moisture and volatile substance were determined by weightlessness method and inorganic impurities was determined by the residue on ignition method. The content of AEE reference substance was calculated by the mass balancemethod. NMR quantification method for AEE was established with determine temperature of 25 ℃,scan times of 16 and the relaxation delay time of 15 s respectively. RESULTS： The results of content determination were 99. 82% by the mass balance method and 99. 55% by the NMR method. Fitting line between peak area ratio and weight ratio of sample AEE to inner standard（ 1,4-dinitrobenzene） ranged from 3 mg to 21 mg with correlative coefficient of 0. 999. Method validation of the NMR about the precision RSD was 0. 04%（ n = 5） and the repeatability RSD was 0. 19%（ n = 5） and the stability of RSD was0. 57%. CONCLUSIONS： Two methods can verify each other and the determination results are basically identical.