Leyssens L, Martens V, Royackers E, Penxten H, Verheyden A, Czech J, Raus J
Laboratory of Drug Analysis, Dr L. Willems-Instituut, Diepenbeek, Belgium.
J Pharm Biomed Anal. 1990;8(8-12):919-27. doi: 10.1016/0731-7085(90)80143-d.
A sample work-up method for gas chromatographic profiling of polyoxyethylene glycol (PEG)-related compounds in pharmaceutical matrices is described. After a short sample clean-up, carbon-oxygen linkages are partially cleaved with 0.07 M boron tribromide in dichloromethane at room temperature. The reaction is stopped after 1 min by addition of 0.01 M HCl. The products are trimethylsilylated and injected onto a WCOT 50 m x 0.25 mm CP-SIL 5 CB fused silica column. Eleven model compounds, representing four common types of PEG-derivatives, have been evaluated by this method. The results show that characteristic profiles can be obtained from PEG-derivatives carrying different functional groups. Minimum detectable amounts are in the range of 200 micrograms.
描述了一种用于药物基质中聚乙二醇（PEG）相关化合物气相色谱分析的样品处理方法。经过简短的样品净化后，在室温下用二氯甲烷中的0.07 M三溴化硼将碳 - 氧键部分裂解。1分钟后通过加入0.01 M HCl停止反应。产物进行三甲基硅烷化处理后注入到一根50 m×0.25 mm WCOT CP - SIL 5 CB熔融石英柱上。通过该方法评估了代表四种常见PEG衍生物类型的11种模型化合物。结果表明，可以从带有不同官能团的PEG衍生物中获得特征图谱。最低检测量在200微克范围内。
