加替沙星的紫外、荧光分光光度法和高效液相色谱法测定  

Spectrophotometric, spectrofluorimetric and reversed-phase high-performance liquid chromatographic methods for determination of gatifloxacin in its capsule

作　　者：于素华[1] 孟文静[1] 陆婷婷[1] 杨功俊[1] 

机构地区：[1]扬州大学化学化工学院,江苏扬州225002

出　　处：《扬州大学学报（自然科学版）》2008年第2期40-44,共5页Journal of Yangzhou University：Natural Science Edition

基　　金：生命分析化学教育部重点实验室基金资助项目(KLACLS07005);物理化学国家重点学科培育点资助项目

摘　　要：采用紫外分光光度法、荧光分光光度法和反相高效液相色谱法测定胶囊中加替沙星含量.在0.04mol·L-1HAc-NaAc缓冲溶液(pH=4.3)中直接根据加替沙星的紫外吸收光谱进行测定;于0.04mol·L-1HAc-NaAc缓冲溶液(pH=4.3)和0.014mol·L-1十二烷基磺酸钠(SDS)体系中,以330nm作为激发波长,在484nm处测定其荧光强度;以VP-ODS为色谱柱(150mm×4.6mm,5.0μm),柱温为35℃,流动相为V(CH3OH)∶V(H2O)=45∶55(用醋酸调节pH至3.5),流速为1.0mL·min-1,检测波长为292nm,建立了测定加替沙星的反相高效液相色谱法.3种方法对胶囊中加替沙星含量5次测定结果的平均值分别为98%,96%,102%,RSD分别为2.5%,2.7%,1.9%,表明该方法可用于加替沙星制剂的质量控制.Three methods, including spectrophotometry, spectrofluorimetry and reversed-phase highperformance liquid chromatography, are described for determination of gatifloxacin in its capsules. The spectrophotometric method is based on measurement of its native absorption in 0.04 mol · L^-1HAc- NaAc buffer solution （pH= 4.3）. The specrtofluorimetric method is based on the determination of its fluorescence intensity in 0.04 mol· L^-1 HAc-NaAc buffer solution （pH= 4.3） and 0. 014 mol · L^-1 SDS at the emission wavelength Of 484 nm upon the excitation at the wavelength of 330 nm. The third method is based on the reversed-phase high-performance liquid chromatographic determination of gatifloxacin using a VP ODS column （150 mm × 4.6 mm, 5.0 μm） maintained at 35 ℃, with the mobile phase of V（CH3OH） ： V（H2O）=45 ： 55 （pH 3.5, adjusted by acetic acid） at the flow-rate of 1.0 mL · min^-1, and UV detection at 292 nm. The three methods are applied to determine the content of gatifloxacin capsules. The average results of five times obtained by spectrophotometry, spectrofluorimetry and reversed-phase high-performance liquid chromatography are 98%, 96%, and 102%, and RSD are 2.5%, 2.7% and 1.9%, respectively. It manifested that these methods can be used to control the quality of gatifloxacin preparation.

关 键 词：加替沙星 紫外分光光度法 荧光分光光度法 反相高效液相色谱法 胶囊 

分 类 号：O657.3[理学—分析化学] R927.2[理学—化学]