Hengsawas Surasarang Soraya, Florova Galina, Komissarov Andrey A, Shetty Sreerama, Idell Steven, Williams Robert O
a Division of Pharmaceutics , College of Pharmacy, The University of Texas at Austin , Austin , TX , USA.
b School of Medical Biological Sciences , The University of Texas Health Science Center at Tyler , Tyler , TX , USA.
Drug Dev Ind Pharm. 2018 Feb;44(2):184-198. doi: 10.1080/03639045.2017.1371736. Epub 2017 Nov 10.
A caveolin-1 scaffolding domain, CSP7, is a newly developed peptide for the treatment of idiopathic pulmonary fibrosis. To develop a CSP7 formulation for further use we have obtained, characterized and compared a number of lyophilized formulations of CSP7 trifluoroacetate with DPBS and in combination with excipients (mannitol and lactose at molar ratios 1:5, 70 and 140). CSP7 trifluoroacetate was stable (>95%) in solution at 5 and 25 °C for up to 48 h and tolerated at least 5 freeze/thaw cycles. Lyophilized cakes of CSP7 trifluoroacetate with excipients were stable (>96%) for up to 4 weeks at room temperature (RT), and retained more than 98% of the CSP7 trifluoroacetate in the solution at 8 h after reconstitution at RT. The lyophilized CSP7 formulations were stable for up to 10 months at 5 °C protected from moisture. Exposure of the lyophilized cakes of CSP7 to 75% relative humidity (RH) resulted in an increase in the absorbed moisture, promoted crystallization of the excipients and induced reversible formation of CSP7 aggregates. Increased molar ratio of mannitol slightly affected formation of the aggregates. In contrast, lactose significantly decreased (up to 20 times) aggregate formation with apparent saturation at the molar ratio of 1:70. The possible mechanisms of stabilization of CSP7 trifluoroacetate in solid state by lactose include physical state of the bulking agent and the interactions between lactose and CSP7 trifluoroacetate (e.g. formation of a Schiff base with the N-terminal amino group of CSP7). Finally, CSP7 trifluoroacetate exhibited excellent stability during nebulization of formulations containing mannitol or lactose.
窖蛋白-1支架结构域CSP7是一种新开发的用于治疗特发性肺纤维化的肽。为了开发可供进一步使用的CSP7制剂,我们制备、表征并比较了多种CSP7三氟乙酸盐与DPBS以及与辅料(甘露醇和乳糖,摩尔比分别为1:5、70和140)组合的冻干制剂。CSP7三氟乙酸盐在5℃和25℃的溶液中稳定(>95%)达48小时,并且至少耐受5次冻融循环。含有辅料的CSP7三氟乙酸盐冻干饼在室温下长达4周稳定(>96%),在室温复溶8小时后,溶液中保留的CSP7三氟乙酸盐超过98%。冻干的CSP7制剂在5℃防潮条件下长达10个月稳定。将CSP7冻干饼暴露于75%相对湿度(RH)会导致吸收水分增加,促进辅料结晶,并诱导CSP7聚集体可逆形成。甘露醇摩尔比增加对聚集体形成略有影响。相比之下,乳糖显著减少(高达20倍)聚集体形成,在摩尔比为1:70时明显达到饱和。乳糖使CSP7三氟乙酸盐在固态中稳定的可能机制包括填充剂的物理状态以及乳糖与CSP7三氟乙酸盐之间的相互作用(例如与CSP7的N端氨基形成席夫碱)。最后,CSP7三氟乙酸盐在含有甘露醇或乳糖的制剂雾化过程中表现出优异的稳定性。