Elshaboury Salwa R, Mohamed Niveen A, Ahmed Sameh, Farrag Shereen
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut 71526, Egypt.
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut 71526, Egypt Pharmacognosy and Pharmaceutical Chemistry Department, College of Pharmacy, Taibah University, Al Madinah AlMunawarah 30001, Kingdom of Saudi Arabia
J Chromatogr Sci. 2016 Mar;54(3):419-28. doi: 10.1093/chromsci/bmv159. Epub 2015 Nov 3.
A simple, efficient and reliable ion-pair chromatography (IPC) method was developed and validated for the determination of some H2 receptor antagonists including ranitidine (RAN), nizatidine (NIZ) and famotidine (FAM). The use of IPC separations provided improved peak resolution with good peak shape in short analysis time and augmented method selectivity compared with the frequently used RP-C18 methods. A simple isocratic mode with mobile phase containing acetonitrile and 20 mM acetate buffer (50 : 50, v/v) containing 20 mM sodium dodecyl sulfate was used for separation. The flow rate was set at 1.0 mL min(-1), and the effluent was monitored by UV detector at 280 nm FAM and 320 nm for NIZ and RAN. The method was validated in accordance with International Conference on Harmonization guidelines and shown to be suitable for intended applications. The limits of detections and quantitations were 0.008-0.011 and 0.025-0.033 µg mL(-1), respectively. The proposed IPC method was successfully applied for the determination of pharmaceutical dosage forms without prior need for separation. Additionally, the developed method was applied for the determination of RAN in rabbit plasma using NIZ as the internal standard. The method entailed direct injection of the plasma samples after deproteination using methanol. Finally, the proposed IPC method was applied successfully in a pharmacokinetic study for RAN in rabbits after a single oral dose of RAN.
开发并验证了一种简单、高效且可靠的离子对色谱法（IPC），用于测定包括雷尼替丁（RAN）、尼扎替丁（NIZ）和法莫替丁（FAM）在内的一些H2受体拮抗剂。与常用的反相C18方法相比，IPC分离在短分析时间内提供了更好的峰分辨率和良好的峰形，并提高了方法的选择性。采用简单的等度洗脱模式，流动相为含乙腈和20 mM乙酸盐缓冲液（50 : 50，v/v）且含有20 mM十二烷基硫酸钠的溶液进行分离。流速设定为1.0 mL min(-1)，流出物通过紫外检测器在280 nm处监测FAM，在320 nm处监测NIZ和RAN。该方法按照国际协调会议指南进行了验证，结果表明适用于预期应用。检测限和定量限分别为0.008 - 0.011和0.025 - 0.033 µg mL(-1)。所提出的IPC方法成功应用于药物剂型的测定，无需事先分离。此外，所开发的方法以NIZ为内标用于测定兔血浆中的RAN。该方法包括使用甲醇进行蛋白沉淀后直接进样血浆样品。最后，所提出的IPC方法成功应用于单次口服RAN后兔体内RAN的药代动力学研究。
