D'Souza Susan, Faraj Jabar A, Dorati Rossella, DeLuca Patrick P
University of Kentucky College of Pharmacy, Lexington, Kentucky, 40536, USA,
AAPS PharmSciTech. 2014 Jun;15(3):530-41. doi: 10.1208/s12249-013-0052-0. Epub 2014 Feb 12.
Accelerated in vitro release testing methodology has been developed as an indicator of product performance to be used as a discriminatory quality control (QC) technique for the release of clinical and commercial batches of biodegradable microspheres. While product performance of biodegradable microspheres can be verified by in vivo and/or in vitro experiments, such evaluation can be particularly challenging because of slow polymer degradation, resulting in extended study times, labor, and expense. Three batches of Leuprolide poly(lactic-co-glycolic acid) (PLGA) microspheres having varying morphology (process variants having different particle size and specific surface area) were manufactured by the solvent extraction/evaporation technique. Tests involving in vitro release, polymer degradation and hydration of the microspheres were performed on the three batches at 55°C. In vitro peptide release at 55°C was analyzed using a previously derived modification of the Weibull function termed the modified Weibull equation (MWE). Experimental observations and data analysis confirm excellent reproducibility studies within and between batches of the microsphere formulations demonstrating the predictability of the accelerated experiments at 55°C. The accelerated test method was also successfully able to distinguish the in vitro product performance between the three batches having varying morphology (process variants), indicating that it is a suitable QC tool to discriminate product or process variants in clinical or commercial batches of microspheres. Additionally, data analysis utilized the MWE to further quantify the differences obtained from the accelerated in vitro product performance test between process variants, thereby enhancing the discriminatory power of the accelerated methodology at 55°C.
已开发出加速体外释放测试方法,作为产品性能指标,用作临床和商业批次可生物降解微球放行的鉴别性质量控制(QC)技术。虽然可生物降解微球的产品性能可通过体内和/或体外实验进行验证,但由于聚合物降解缓慢,这种评估可能特别具有挑战性,导致研究时间延长、劳动量大且费用高。通过溶剂萃取/蒸发技术制备了三批形态各异(具有不同粒径和比表面积的工艺变体)的亮丙瑞林聚乳酸-羟基乙酸共聚物(PLGA)微球。在55°C下对这三批微球进行了体外释放、聚合物降解和微球水合测试。使用先前推导的称为修正威布尔方程(MWE)的威布尔函数修正形式分析了55°C下的体外肽释放。实验观察和数据分析证实了微球制剂批次内和批次间出色的重现性研究,证明了55°C加速实验的可预测性。加速测试方法还成功地区分了具有不同形态(工艺变体)的三批微球之间的体外产品性能,表明它是鉴别临床或商业批次微球中产品或工艺变体的合适QC工具。此外,数据分析利用MWE进一步量化了工艺变体之间加速体外产品性能测试获得的差异,从而增强了55°C加速方法的鉴别能力。