摘要: |
(目的)本文旨在联合使用质量平衡法与差示扫描量热法2种定值方法测定非班太尔对照品的含量。(方法)采用高效液相色谱法测定非班太尔的纯度,采用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;采用差示扫描量热法对非班太尔对照品含量加以佐证。(结果)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99.66%。(结论)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,2种方法能够更好地保证非班太尔对照品赋值的准确性。 |
关键词: 非班太尔 对照品定值 质量平衡法 差示扫描量热法 |
DOI: |
投稿时间:2021-03-14修订日期:2021-08-20 |
基金项目: |
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MA Qiu-ran, ZHANG Lu, DONG Ling-ling, FAN Qiang* |
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(China institute of veterinary drug control) |
Abstract: |
(Objective)To determine the content of febantel reference substance by the two methods including mass balance and differential scanning calorimetry (DSC). (Method)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 the content of febantel reference substance was verified by differential scanning calorimetry. (Result)The results of mass balance method and differential scanning calorimetry were of equal precision by Cochran test. Thus, the arithmetic average value was 99.66%, which was taken as the final content of febantel reference substance. (Conclusion)The assignment results of mass balance and differential scanning calorimetry were consistent, and two methods can guarantee the accuracy of the assignment. |
Key words: febantel assignment of reference substance mass balance differential scanning calorimetry uncertainty |