差示扫描量热法对芝麻酚纯度标准物质的定值

DEFINING VALUE OF SESAMOL PURITY REFERENCE MATERIALS BY DIFFERENTIAL SCANNING CALORIMETRY

建立了采用差示扫描量热法对芝麻酚纯度标准物质的定值及不确定度评价的数学模型、有效检测技术和分析方法。采用差示扫描量热法测量芝麻酚样品纯度的实验条件为升温速率3.0 K/min,称样量3.4～4.7 mg,炉内气体为静态空气。对通过均匀性检验和长期稳定性考察的芝麻酚纯度标准物质进行定值和不确定度评价,同时采用高效液相色谱法进行实验结果验证。芝麻酚在3.4～4.7 mg范围内与峰面积呈线性关系(r2=0.9992,n=6);方法精密度为0.89%(n=6);采用差示扫描量热法及建立的数学模型对芝麻酚纯度标准物质定值及不确定度评价结果为99.46%±0.09%(k=2,P=0.95)。HPLC法测定纯度平均值为99.53%。建立的差示扫描量热法检测技术可实现对芝麻酚纯度标准物质的定值及不确定度评价,该检测分析方法具有简便、快速、准确的特点。

The analytical method and mathematical model for purity and uncertainty evaluation of sesamol purity reference materials were established. The purity of the substance was measured by the DSC. The experimental conditions were listed below： the heating rate at 3.0 K / min, the sample weight was 3.4--4.7 mg, furnace gas as a static air. The purity and uncertainty value of sesamol was determined, which through the uniformity test and long-term stability inspection. The purity value results were verified by HPLC method. The calibration curves showed good linearity （r2=0.9992, n=6） within tested mass ranges of sesamol （3.4-4.7 mg）. The RSD was 0.89%（n=6）. The purity value of sesamol purity reference materials determined by DSC was 99.46% ＋ 0.09%（k=2, P=0.95）, and 99.53% by HPLC. The differential scanning calorimetry method developed in this study was validated to be simple, rapid, accurate, reliable, and was successfully applied to the purity and uncertainty evaluation of sesamol purity reference materials.