Venugopal Kolachina, Snehalatha Movva, Bende Girish, Saha Ranendra
Birla Institute of Technology and Science, Pharmacy Group, FD III and EDD, BITS Pilani Rajasthan.
J Chromatogr Sci. 2007 Apr;45(4):220-5. doi: 10.1093/chromsci/45.4.220.
A new, simple, and sensitive ion-pair reverse-phase liquid chromatographic method is developed and validated for the estimation of 1-cyclopropyl-6-fluoro-8-methoxy-7-(3-methylpiperazin-1-yl)-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid (gatifloxacin) in bulk and formulations using a UV detector under isocratic conditions. The selected mobile phase consists of the aqueous phase (a 25 mM citrate buffer comprising of 10mM cationic and anionic pairing agents, pH adjusted to 3.5) and acetonitrile (52:48%, v/v). The selected wavelength is 292 nm. Retention time of gatifloxacin is 5.2 min. The linearity range is found to be 50 to 1000 ng/mL (the regression equation is area = 105.5 x concentration in ng/mL--695.8), and the regression coefficient is 0.9996. Validation results demonstrate accuracy, precision, and reproducibility (relative standard deviation < 3%) of the method. The detection and quantitation limits are found to be 6.50 and 17.38 ng/mL, respectively. The method is successfully used for the estimation of gatifloxacin in a variety of dosage forms, and the results are in good agreement with the label claims.
开发并验证了一种新的、简单且灵敏的离子对反相液相色谱法，用于在等度条件下使用紫外检测器测定原料药和制剂中的1-环丙基-6-氟-8-甲氧基-7-(3-甲基哌嗪-1-基)-4-氧代-1,4-二氢喹啉-3-羧酸（加替沙星）。所选流动相由水相（含10 mM阳离子和阴离子配对剂的25 mM柠檬酸盐缓冲液，pH调至3.5）和乙腈（52:48%，v/v）组成。所选波长为292 nm。加替沙星的保留时间为5.2分钟。线性范围为50至1000 ng/mL（回归方程为面积 = 105.5×浓度（ng/mL） - 695.8），回归系数为0.9996。验证结果证明了该方法的准确性、精密度和重现性（相对标准偏差<3%）。检测限和定量限分别为6.50和17.38 ng/mL。该方法成功用于多种剂型中加替沙星的测定，结果与标签标示量良好吻合。
