Haidar Ahmad Imad A, Blasko Andrei
Analytical Research and Development, Novartis Pharmaceuticals Corporation.
Analytical Research and Development, Novartis Pharmaceuticals Corporation;
J Vis Exp. 2017 Aug 11(126):56175. doi: 10.3791/56175.
The aim of this work is to identify the parameters that affect the recovery of pharmaceutical residues from the surface of stainless steel coupons. A series of factors were assessed, including drug product spike levels, spiking procedure, drug-excipient ratios, analyst-to-analyst variability, intraday variability, and cleaning procedure of the coupons. The lack of a well-defined procedure that consistently cleaned the coupon surface was identified as the major contributor to low and variable recoveries. Assessment of cleaning the surface of the coupons with clean-in-place solutions (CIP) gave high recovery (>90%) and reproducible results (Srel≤4%) regardless of the conditions that were assessed previously. The approach was successfully applied for cleaning verification of small molecules (MW <1,000 Da) as well as large biomolecules (MW up to 50,000 Da).
这项工作的目的是确定影响从不锈钢试片表面回收药物残留的参数。评估了一系列因素，包括药品加标水平、加标程序、药物与辅料比例、分析人员之间的差异、日内差异以及试片的清洗程序。缺乏始终如一地清洁试片表面的明确程序被确定为回收率低且变化不定的主要原因。使用在位清洗溶液（CIP）对试片表面进行清洗的评估显示，无论之前评估的条件如何，回收率都很高（>90%）且结果具有可重复性（相对标准偏差≤4%）。该方法已成功应用于小分子（分子量<1000 Da）以及大分子（分子量高达50000 Da）的清洗验证。
