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各位蒲友:
针对于原料药的混合,大家的取样方法一般是怎么样的呢??(针对于单锥,双锥),非常感谢??下文的被取消的指南虽然是针对的是制剂的,但是其中涉及到取样策略(比如取≥10个sample locations并在每个取样点取3个replicate samples)不知道是否能用到API过程中,本人没有找到相关的API混合的相关的指南,求指导。
15. FDA withdrew its draft guidance for industry on Powder Blends and Finished Dosage Units—Stratified In-Process Dosage Unit Sampling and Assessment. What were the Agency’s major concerns with this guidance?
FDA’s major concern was that sections V and VII of the withdrawn draft guidance no longer represented the Agency’s current thinking, as explained below.
Section V (Exhibit/Validation Batch Powder Mix Homogeneity) recommended that at least 3 replicate samples be taken from at least 10 locations in the powder blender, but that only 1 of the 3 replicates be evaluated to assess powder blend uniformity. The Agency currently recommends that all replicate samples taken from various locations in the blender be evaluated to perform a statistically valid analysis. (原先的按照决策树的是取至少10个点,每个点取三个样,然后测定3个样中的一个样用于评价,其他两个样用于调查,agency现在推荐所有的取样均进行测定评估混合有效性)This analysis can demonstrate that variability attributable to sample location is not significant and that the powder blend is homogenous. Statistical tools are available to ascertain both the number of replicates and the number of sampling locations across the blender that should be analyzed to conduct a valid analysis. (这种3replicate sampless检测能够证明取样位置的差异性not significant,但是关于每个点的取样数以及取样位置数需要使用统计的方法确定)
Section VII (Routine Manufacturing Batch Testing Methods) acceptance criteria designated to the Standard Criteria Method and the Marginal Criteria Method were based upon the limits published in the United States Pharmacopeia (USP) General Chapter <905> Uniformity of Dosage Units. However, the procedures and acceptance criteria in General Chapter <905> are not a statistical sampling plan and so the results of the procedures should not be extrapolated to larger populations. Therefore, because the procedure and acceptance criteria prescribed in section VII provided only limited statistical assurance that batches of drug products met appropriate specifications and statistical quality control criteria, FDA no longer supports their use for batch release. Currently, there are several standard statistical practices that, if used correctly, can help to ensure compliance with CGMP regulations, including 21 CFR 211.110, 21 CFR 211.160, and 21 CFR 211.165.
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