Eli Lilly Canada Inc, 3650 Danforth Ave, Toronto, Ontario M1N 2E8, Canada.
J Pharm Biomed Anal. 2010 Jun 5;52(2):316-9. doi: 10.1016/j.jpba.2010.01.012. Epub 2010 Jan 18.
During development of the residual solvent method using headspace-GC for a drug substance, an unexpected peak was observed in the chromatography. GC-MS analysis confirmed the unknown peak identity as isobutylene. An understanding of the source of the isobutylene was required in order to develop appropriate impurity and residual solvent control strategies for the drug substance. The experiments performed to determine the source of the isobutylene peak observed in the headspace-GC chromatography and how the tert-butoxycarbonyl (BOC) de-protection step used in the drug substance synthesis contributes to its observation are discussed.
在采用顶空-GC 法对药物进行残留溶剂研究的过程中，色谱图中出现了一个意外的峰。GC-MS 分析证实该未知峰为异丁烯。为了对药物制定适当的杂质和残留溶剂控制策略，需要了解异丁烯的来源。本文讨论了确定顶空-GC 色谱中观察到的异丁烯峰来源的实验，以及药物合成中使用的叔丁氧羰基（BOC）脱保护步骤如何导致该峰的出现。
