非班太尔对照品的定值研究

Assignment Study of Febantel Chemical Reference Substance

采用质量平衡法与差示扫描量热法两种不同原理的定值方法测定非班太尔对照品的含量,并评估研制过程中引入的不确定度。采用高效液相色谱法测定非班太尔对照品的纯度,卡尔费休氏容量滴定法、炽灼残渣检查法、气相色谱法分别测定其水分、灰分和残留溶剂,由质量平衡法公式计算非班太尔对照品的含量;差示扫描量热法对非班太尔对照品含量加以佐证;趋势分析法对非班太尔对照品的均匀性和稳定性进行考察;采用不确定度评价方法对定值结果进行不确定度评价。结果表明:质量平衡法和差示扫描量热法测定结果经科克伦判定互为等精度,取其算术平均值作为最终定值结果,即非班太尔对照品含量为99.7%,扩展不确定度为0.3%(k=2),均匀性和稳定性均符合要求。质量平衡法与差示扫描量热法对非班太尔对照品的定值结果基本一致,两种方法能够更好地保证非班太尔对照品赋值的准确性。

To determine the content of febantel reference substance by the two methods including mass balance and differential scanning calorimetry(DSC),the chromatographic purity of febantal reference substance was determined by HPLC method.Moisture,ignition residue and residual solvents were determined by Karl-Fishier-titration method,sulfated ash test method and gas chromatography,respectively.Then the content of febantel reference substance was calculated by mass balance method,and verified by differential scanning calorimetry.The homogeneity and stability were investigated by trend analysis.The results of mass balance method and differential scanning calorimetry were of equal precision by Cochran test.Thus,the arithmetic average value was 99.7%,the expand uncertainty was 0.3%(k=2),the homogeneity and stability meet the specification.The assignment results of mass balance and differential scanning calorimetry were consistent,and two methods can guarantee the accuracy of the assignment.