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目的对溶出仪自动取样系统进行校准。方法采用经机械校准合格的溶出仪,对D、K 2种自动取样系统的取样体积、取样时间进行校准,对溶出仪采用自动与手动取样时的整机性能进行校准,并比对连续多个取样时间点自动与同时手动取样的水杨酸片的溶出量以计算偏差。结果溶出仪机械性能校准合格,自动与手动取样时溶出仪的整机性能校准合格,D、K 2种自动取样系统体积误差SS≤±2%,精密度SR≤3%,取样值滤过时间均<30 s,表明取样快速,取样体积准确、精密;D自动取样系统与手动取样溶出的比值R的均值在篮法和桨法下均<100%,且有部分点<95%,而K自动取样系统的R均值约为98%~102%,表明D系统存在一定偏差,而K系统无明显偏差。结论应对自动取样系统进行校准,对其偏差进行评估,制定可接受标准,建议体积误差SS≤±5%,精密度SR≤5%,取样值滤过时间均<30 s;溶出量≤50%的点R均值为95%~105%,R的相关标准偏差≤5%;溶出量>50%的点R均值为97%~103%,R的相对标准偏差≤5%。
Objective To calibrate the dissolution instrument automatic sampling system. Methods The sample volume and sampling time of D and K automatic sampling systems were calibrated by using a qualified dissolution apparatus. The performance of the dissolution apparatus was calibrated automatically and manually, Sampling time points automatically and simultaneously manually sampled salicylic acid tablets to calculate the amount of dissolution. Results The mechanical properties of the dissolution apparatus passed the calibration. The performance of the dissolution apparatus was qualified both automatically and manually. The volume errors of D and K automatic sampling systems were SS≤ ± 2% and the precision was SR≤3%. The filtration time All <30 s, indicating that the sampling was rapid and the sampling volume was accurate and accurate. The average value of the ratio R between the D automatic sampling system and the manual sample dissolution was <100% under the basket method and the paddle method, with some points <95% The average value of R in the automatic sampling system is about 98% -102%, indicating that there is a certain deviation in the D system and no obvious deviation in the K system. Conclusion The automatic sampling system should be calibrated, the deviation should be evaluated and the acceptable standard should be established. The recommended volume error is SS≤ ± 5%, precision SR≤5%, sample filtration time <30 s, dissolution rate≤50% The mean R of the spots was 95% -105%, the relative standard deviation of R was ≤5%, the average of the spot R of dissolution> 50% was 97% -103%, and the relative standard deviation of R was ≤5%.