HPLC法测定盐酸多西环素及其制剂含量和有关物质  

HPLC determination of doxycycline hydrochloside and its related substunces

作　　者：袁耀佐[1] 张玫[1] 钱文[1] 杨志明 赵恂[1] 

机构地区：[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

出　　处：《药物分析杂志》2010年第12期2304-2310,共7页Chinese Journal of Pharmaceutical Analysis

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 solve the blocking problem of the current official pharmacopeia and establish a new HPLC method for the determination of doxycycline hyclate and its preparations.Methods：The meithod was carried using a column packed with octadecysilane bonded silica gel and a mixture of a buffer solution containing 100 volumes of 0.25 mol·L-1 ammonium acetate solution,10 volumes of 0.1 mol·L-1 ethyldiaminetetraacetic acid disodium salt solution and 1 volume of triethyamine adjusted pH to 8.8 with glacial acetic acid-acetonitrile（85∶15）as the mobile phase,and with a column temperature of 35 ℃,a detection wavelength of 280 nm,a flow rate of 1 mL·min-1,and the injection volume was 20 μL.Results：The blocking problem of the current official pharmacopeia was overcame and a good resolution with baseline separation was obtained by the established chromatographic system.The linear range was 0.07-122.56 μg·mL-1（r=1.0）,the limit of detection was 0.016 μg·mL-1,and the limit of quantity was 0.063 μg·mL-1.The average recovery data of tablet and capsule was 99.2%（n=9,RSD=0.2%）and 99.4%（n=9,RSD=0.2%）,respectively.This chromatographic system can be applied to the determination of oxytetracycline,tetracycline,chlorotetracycline,minocycline and metacycline by adjusting the mobile phase ratio of acetate buffer and acetonitrile.Conclusions：The established method is better than the methods of ChP 2005,USP 31,BP 2008,EP 6.0 and JPⅩⅤ and was adopted by ChP 2010.

关 键 词：盐酸多西环素 高效液相色谱法 含量测定 有关物质 

分 类 号：R917[医药卫生—药物分析学]