溶出仪自动取样系统的校准

程开生; 丁竞男; 陈建斌

doi:10.13748/j.cnki.issn1007-7693.2017.11.020

溶出仪自动取样系统的校准

Verification of Dissolution Apparatus Auto Sampling System

摘要

摘要: 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S_S ≤ ±2%，精密度S_R ≤ 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S_S ≤ ±5%，精密度S_R ≤ 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%。

Abstract: OBJECTIVE To evaluate and verification the dissolution apparatus auto sampling system. METHODS Employed mechanical qualified dissolution apparatus, evaluate the auto sampling system D, K based on the accuracy(S_S) and precision(S_R) of sampling volume and time of sampling to filter. Verificate the overall performance of dissolution apparatus based on the dissolution of salicylic acid tablets. The ratio of auto to manual in three sampling time points was calculated. RESULTS D & K auto sampling system sampling accuracy(S_S) were within ±2% and precision(S_R) were ≤ 3%. The sampling time <30 s. It was suggested the D & K auto sampling system were fast, accurate and precisely. The average ratio of auto D to manual were <100%, sometimes were <95%, which the ratio of auto K was in the range of 98%-102%. The results showed that there was a certain deviation in D system, but there was no obvious deviation in K system. CONCLUSION The auto sampling system should be verificated. It is suggested the acceptal criteria is:sampling time ≤ 30 s, S_S ≤ ±5%, S_R ≤ 5%; Average of R is in the range of 95%-105% and RSD ≤ 5% at time points with ≤ 50% dissolved, which is 97%-103% and RSD ≤ 5% for time points >50%.

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