Arayne M Saeed, Sultana Najma, Zuberi M Hashim, Siddiqui Farhan Ahmed
Department of Chemistry, University of Karachi, Karachi-75270, Pakistan.
J Chromatogr Sci. 2010 Oct;48(9):721-5. doi: 10.1093/chromsci/48.9.721.
A new, simple, and reliable reversed-phase high-performance liquid chromatographic method has been developed and validated for the simultaneous determination of metformin (Metf), cimetidine (Cimt), famotidine (Famt), and ranitidine (Rant) in their synthetic mixtures and tablet formulations. These drugs were separated on a Purospher Star RP18 endcapped (250 mm × 4.6 mm i.d.) column packed with 5-μm particles. The mobile phase, optimized through an experimental design, consisted of methanol-water-triethylamine (20:80:0.05), whose pH was adjusted to 3.0 with phosphoric acid (85%) pumped at a flow rate of 1.0 mL/min. UV detection was performed at 229 nm. The method was validated in the sample concentration range of 5-25 μg/mL for all the drugs, where it demonstrated good linearity with r = 0.9998, 0.9979, 0.9997, and 0.9987 (n = 6), respectively. For independent 100% level samples, the intra-day and inter-day precision was in the range i.e. < 2.0 for all the drugs. The method demonstrated robustness, resisting to small deliberate changes in pH, flow rate, and composition (organic:aqueous ratio) of the mobile phase. The limit of detection values were 0.071, 0.116, 0.134, and 0.110 μg/mL, while the limit of quantitation were 0.217, 0.352, 0.405, and 0.368 μg/mL for Metf, Cimt, Famt, and Rant, respectively. The applicability of the method was demonstrated by determining the drug content in pharmaceutical formulations, where it exhibited good performance.
已开发并验证了一种新的、简单且可靠的反相高效液相色谱法，用于同时测定合成混合物和片剂制剂中的二甲双胍（Metf）、西咪替丁（Cimt）、法莫替丁（Famt）和雷尼替丁（Rant）。这些药物在填充有5-μm颗粒的Purospher Star RP18封端（250 mm×4.6 mm内径）柱上分离。通过实验设计优化的流动相由甲醇-水-三乙胺（20:80:0.05）组成，用磷酸（85%）将其pH调节至3.0，以1.0 mL/min的流速泵送。在229 nm处进行紫外检测。该方法在所有药物的5-25μg/mL样品浓度范围内进行了验证，在此范围内分别显示出良好的线性，r = 0.9998、0.9979、0.9997和0.9987（n = 6）。对于独立的100%水平样品，所有药物的日内和日间精密度范围均<2.0。该方法表现出稳健性，能抵抗流动相pH、流速和组成（有机相：水相比例）的微小故意变化。二甲双胍、西咪替丁、法莫替丁和雷尼替丁的检测限分别为0.071、0.116、0.134和0.110μg/mL，定量限分别为0.217、0.352、0.405和0.368μg/mL。通过测定药物制剂中的药物含量证明了该方法的适用性，其表现良好。
