盐酸多西环素ChP 2015标准检测的紧邻主成分后杂质的制备及鉴定

发布时间：2018-09-18 12:29

【摘要】：目的:制备盐酸多西环素中国药典2015年版(Ch P 2015)标准检测的紧邻主峰后杂质,并鉴定其结构。方法:以盐酸多西环素成盐用母液为对象,采用室温条件下半制备液相色谱分离纯化杂质;色谱条件:采用Synergi C_(18)(50 mm×250 mm,10μm)色谱柱,以0.1%三氟乙酸水溶液(A)-0.1%三氟乙酸乙腈溶液(B)为流动相,线性梯度洗脱(A-B):0.0 min(85∶15)→40.0 min(60∶40)→40.5 min(85∶15)?50.0 min(85∶15),流速为80 m L·min~(-1);254 nm检测收集目标组分,旋转蒸发去除有机溶剂,冷冻干燥制得目标杂质;采用盐酸多西环素Ch P 2015标准中有关物质检查的高效液相色谱法确证制得物质为目标杂质并采用归一化方法测定其纯度;采用光谱综合分析等手段确证其结构。结果:制得目标杂质纯度为98.7%,结构确证为2-乙酰-2-脱氨甲酰多西环素(即EP 8.0中的盐酸多西环素杂质F),在有关物质测定用供试品溶液中添加该杂质后,多西环素后相邻峰面积显著增加。结论:盐酸多西环素Ch P 2015标准检测的紧邻主峰后杂质经制备色谱分离并成功鉴定,该结论被Ch P 2015采用。
[Abstract]:Aim: to prepare doxycycline hydrochloride (Ch P 2015) and identify its structure. Methods: the impurities were separated and purified by semi-preparative liquid chromatography at room temperature, and the chromatographic conditions were as follows: Synergi C18 (50 mm 脳 250 mm,10 渭 m) column. Using 0.1% trifluoroacetic acid aqueous solution (A) -0.1% trifluoroacetic acid acetonitrile solution (B) as mobile phase, linear gradient elution (A-B) 0.0 min (85:15) 40.0 min (60:40) 40.5 min (85:15) 50.0 min (85:15), flow rate 80ml min~ (-1) 254nm detection and collection target group, rotating evaporation to remove organic solvent, The target impurity was prepared by freeze-drying, and the purity of the substance was determined by normalized method by high performance liquid chromatography (HPLC) about substance examination in Ch P 2015 standard of doxycycline hydrochloride. The structure was confirmed by means of spectral comprehensive analysis. Results: the purity of the target impurity was 98.7 and the structure was confirmed as 2-acetyl-2-decarbamicyloxycycline (F), the dopicycline hydrochloride impurity in EP 8.0, which was added to the sample solution for the determination of related substances. The area of adjacent peaks increased significantly after doxycycline. Conclusion: the impurities of doxycycline hydrochloride Ch P 2015 were separated by preparative chromatography and identified by Ch P 2015.
【作者单位】：南京理工大学医院;江苏省食品药品监督检验研究院;中国药科大学药物化学教研室;常州制药厂有限公司;中国医药城公共平台服务中心;
【分类号】：R943;R927

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