氟非尼酮光聚合产物的确认与检测
Confirmation and quality control of a photoploymerized substance in fluorofenidone
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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，5 μm），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。Abstract: 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 C18column (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.
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Keywords:
- fluorofenidone /
- photoploymerized substance /
- synthesis /
- characterization /
- qualtity control
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