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利用量热滴定法测定了盐酸普萘洛尔及其制剂的含量,讨论了分析条件及其影响因素。平均回收率为99.76%、变异系数为0.47%.本文曾经在《第五届全国STTT会议》上宣读。指示反应终点,因此反应器皿中溶液初始温度与标准溶液的温度应该均恒一致。本实验是在恒温25”O下进行的。3.1.2绝热反应体系为一镀银的玻璃真空圆瓶(约100。l),外面用绝热材料包裹起来,用玻璃棒搅拌,用热敏电阻作感温元件,量热器只与玻璃接触,热量损失极小。另外,本法并不测定反应热的绝对值,因而对绝热可以适当放宽。3.1.3浓度当玻璃器皿及内容液体的容积固定后,热效应的变化仅依赖于反应物与产物的量,样品的浓度根据药典配制。为消除稀释热的影响,样品的浓度与标准溶液的浓度比为1:50。3.1.4稳定性实验:取0.3995gi原料药制成一定浓度的溶液,在25”O下放置1、2、3、4h,分别测定其含量,结果无甚影响。3二2’回收率试验:‘精称互原料药适量,配成一定浓度的溶液,依样品测定方法操作,测得平均回收率为99.76%,变异系数为0.47%。3.3量热滴定法与药典法比较:3.3·11原料药的量热滴定法与中国药典法比较,见表1。3·3.2盐酸普获洛
The contents of propranolol hydrochloride and its preparations were determined by calorimetric titration. The conditions for the analysis and the influencing factors were discussed. The average recovery was 99.76% with a coefficient of variation of 0.47%. This article was read at the Fifth National STTT Conference. The end of the reaction is indicated, so the initial temperature of the solution in the reaction vessel should be consistent with the temperature of the standard solution. The experiment was carried out at a constant temperature of 25 “O .3.1.2 adiabatic reaction system for a silver-coated glass vacuum round bottle (about 100.l), wrapped with insulating material outside, stirred with a glass rod, hot Sensitive resistance as a temperature sensing element, the calorimeter is only in contact with the glass, the heat loss is minimal.In addition, this law does not determine the absolute value of the reaction heat, so the insulation can be properly relaxed.3.1.3 Concentration When the glassware and After the volume of the content liquid is fixed, the change of the thermal effect depends only on the amount of the reactants and products, and the concentration of the sample is prepared according to the Pharmacopoeia. To eliminate the influence of the dilution heat, the concentration ratio of the sample to the standard solution is 1: 50.3. 1.4 Stability Experiment: Take 0.3995gi raw material drug solution made a certain concentration, placed in 25 ”O 1,2,3,4 h, respectively, the determination of its content, the results had little effect. 3 2 2 ’recovery test:’ accurate mutual drug stock amount, dubbed a certain concentration of the solution, according to sample determination method of operation, the measured average recovery was 99.76%, coefficient of variation of 0.47%. 3.3 Comparison of calorimetry and pharmacopoeia: 3.3 · 11 calorimetric titration of raw materials compared with the Chinese Pharmacopoeia, see Table 1.3 · 3.2 Purcell hydrochloride