摘要
以固态反应制得氟非尼酮的光聚合产物,使用制备色谱分离纯化,通过UV、MS、13C NMR、1H-1H COSY、HMBC、HMBQ对其进行结构确证。建立反相液相色谱法对光照试验中产生的光聚合产物进行检查。色谱条件为:色谱柱为Kromasil C18柱(4.6 mm×250 mm,5μm),流动相为乙腈-0.1%三乙胺(甲磺酸调pH为4.0)(55∶45),流速为1.0 mL/min,柱温为30℃,检测波长为230 nm。结果表明:氟非尼酮对光敏感,在光照下可产生氟非尼酮的二聚体,本研究所建立的HPLC法可灵敏、准确地检测出该物质。
The solid state reaction was used to prepare a photoploymerized substance from fluorofenidone.The photoploymerized substances were separated and purified by pre-HPLC.The spectral analyses,such as UV,MS,13C NMR,1H-1H COSY,HMBC and HMBQ were used to identify the structure of the photoploymerized substances.The HPLC method was established to determine the photoploymerized substance.The chromatographic conditions were as follows：Kromasil C18 column（4.6 mm×250 mm,5 μm） was used and the column temperature was 30 °C.Acetonitrile-water（55 ∶45） containing 0.1% triethylamine,which was adjusted to pH 4.0 by methanesulfonic acid,was used as the mobile phase with a flow rate of 1.0 mL/min;the detection wavelength was 230 nm.The results showed that fluorofenidone is photosensitive and the method is specific and accurate.
出处
《中国药科大学学报》
CAS
CSCD
北大核心
2012年第2期159-163,共5页
Journal of China Pharmaceutical University
基金
国家"重大新药创制"科技重大专项资助项目(No.2009ZX09102-011)~~
关键词
氟非尼酮
光聚合产物
合成
结构确证
质量控制
fluorofenidone
photoploymerized substance
synthesis
characterization
qualtity control
