HPLC法测定盐酸多西环素及其制剂含量和有关物质.docVIP

HPLC 法测定盐酸多西环素及其制剂含量和有关物质 袁耀佐1 ,张玫1 ,钱文1 ,杨志明2 ,赵恂 1 第一作者 Te:l (02586631609;E -m ai :l yuanyaozuo @yahoo . (1.江苏省食品药品检验所,南京210008;2.常州制药厂有限公司,常州213018 摘要 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H PLC 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 25m o l L -1醋酸铵-0 1m ol 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p H 至8 8]-乙腈(85 15为流动相;柱温35!;检测波长280n m,流速1 0mL m i n -1;进样体积20 L 。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 07~122 556 g 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0 063 g 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 01mo l 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。关键词:盐酸多西环素;高效液相色谱法;含量测定;有关物质中图分类号:R 917 文献标识码:A 文章编号:0254-1793(201012-2304-08 HPLC deter m inati on of doxycycli ne hydrochlosi de and its relate d subst unces YUAN Yao-zuo 1 ,Z HANG M ei 1 ,Q I AN W en 1 ,YANG Zhi-m i n g 2 ,Z HAO Xun 1 (1 J i angs u Insti tute f or Food and Drug Con tro,l Nan ji ng 210008,Ch ina ;2 Ch angz hou Phar m aceuti calFactory ,Changz h ou 213018,Ch ina Abst ract Objective :To so lve t h e b lock i n g prob le m of the current o fficial phar m acopeia and estab lish a ne w HPLC m ethod for the deter m i n ation of doxycycline hyclate and its preparations .M ethods :The m eithod w as carried using a co l u m n packed w ith octadecysilane bonded silica ge l and a m i x ture o f a bu ffer so lution con taining 100volum es o f 0 25m o l L -1 a mm on i u m acetate so lution ,10vo l u m es of 0 1m o l L -1 ethy l d ia m inetetraacetic ac i d disod i u m salt solution and 1vo l u m e of triethya m i n e ad j u sted p H to 8 8w ith g l a c i a l acetic ac i d -acetonitrile (85 15as the m o b ile phase ,and w ith a co l u mn te m perature of 35!,a detection w ave length of 280nm ,a flo w rate o f 1mL m i n -1 ,and the i n jecti o n vo l u m e w as 20 L .R esults :The blocking proble m of the curren t officia l phar m acope ia w as over ca m e and a good reso lution w ith baseli n e separati o n w as obtained by