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目的:克服现有色谱流动相易使分析系统堵塞等问题,建立新的盐酸多西环素及其制剂含量和有关物质测定的HPLC方法。方法:用十八烷基硅烷键合硅胶为填充剂,以醋酸盐缓冲液[0.25mol·L-1醋酸铵-0.1mol·L-1乙二胺四醋酸二钠-三乙胺(100∶10∶1),用冰醋酸或氨水调节pH至8.8]-乙腈(85∶15)为流动相;柱温35℃;检测波长280nm,流速1.0mL.min-1;进样体积20μL。结果:新建色谱条件克服了堵塞问题,可使多西环素与相邻杂质基线分离,在0.07～122.556μg.mL-1范围内线性良好(r=1.0),检测限和定量限分别为0.016和0.063μg.mL-1,方法精密度良好,片剂和胶囊的回收率分别为99.2%和99.4%,盐酸多西环素在0.01mol·L-1的盐酸溶液中24h内稳定。该色谱条件微调后,可用于土霉素、四环素、金霉素、米诺环素和美他环素的含量和有关物质的测定。结论:新建色谱条件优于中国药典2005年版、美国药典32版、英国药典2008年版、欧洲药典6.0版和日本药局方XV版,被中国药典2010年版采用。
OBJECTIVE: To overcome the problems of the existing chromatographic mobile phase such as blockage of the analytical system, and to establish a new HPLC method for the determination of doxycycline hyclate and its preparations and related substances. Methods: The octadecylsilane bonded silica gel was used as the filler, and the acetate buffer solution (0.25 mol·L-1 ammonium acetate-0.1 mol·L-1 ethylenediaminetetraacetic acid-triethylamine : 10: 1). The pH was adjusted to 8.8 with acetonitrile or water (85:15). The column temperature was 35 ℃. The detection wavelength was 280 nm and the flow rate was 1.0 mL · min-1. The injection volume was 20 μL. Results: The chromatographic conditions were overcome by the new chromatographic conditions, and the baseline of doxycycline was separated from the adjacent impurities. The linearity was good in the range of 0.07 ~ 122.556μg.mL-1 (r = 1.0). The limits of detection and quantification were 0.016 And 0.063μg.mL-1. The precision of the method was good. The recoveries of tablets and capsules were 99.2% and 99.4%, respectively. The doxycycline hydrochloride was stable in 0.01mol·L-1 hydrochloric acid solution for 24h. The chromatographic conditions after fine-tuning, can be used for oxytetracycline, tetracycline, chlortetracycline, minocycline and mesotrione content and the determination of related substances. Conclusion: The new chromatographic conditions are superior to those of Chinese Pharmacopoeia 2005, American Pharmacopoeia 32, British Pharmacopoeia 2008, European Pharmacopoeia 6.0 and Japanese Pharmacopoeia XV, which were adopted by Chinese Pharmacopoeia 2010 edition.