Kokoletsi Magdalene Xenou, Kafkala Stella, Tsiaganis Michael
R&D Laboratory, Quality Control Department, DEMO SA Pharmaceutical Industry, 21st km National Road Athens-Lamia, 14568 Athens, Greece.
J Pharm Biomed Anal. 2005 Jul 15;38(4):763-7. doi: 10.1016/j.jpba.2005.02.022. Epub 2005 Mar 23.
A selective and accurate high-performance liquid chromatographic method has been developed and validated for the simultaneous determination of ranitidine, methylparaben (MP) and propylparaben (PP) in oral liquids. Samples were purified by solid-phase extraction (SPE) using a copolymeric [poly(divinylbenzene-co-N-vinylpyrrolidone)] sorbent. The chromatographic separation was achieved by HPLC using a mixture of ammonium acetate solution (0.5 M), acetonitrile and methanol as the mobile phase with gradient elution, a Nucleosil C18 column and UV detection at 254 nm. The method was validated with respect to linearity, precision, accuracy, selectivity, and robustness. All the parameters examined met the current recommendations for bioanalytical method validation. The method was found to be applicable to routine analysis (assays and stability tests) of active compound (ranitidine) and preservatives (MP and PP).
已开发并验证了一种选择性和准确性高的高效液相色谱法，用于同时测定口服液中的雷尼替丁、对羟基苯甲酸甲酯（MP）和对羟基苯甲酸丙酯（PP）。样品通过使用共聚[聚（二乙烯基苯-co-N-乙烯基吡咯烷酮）]吸附剂的固相萃取（SPE）进行纯化。采用高效液相色谱法，以醋酸铵溶液（0.5M）、乙腈和甲醇的混合物为流动相进行梯度洗脱，使用Nucleosil C18柱，并在254nm处进行紫外检测，实现了色谱分离。该方法在线性、精密度、准确度、选择性和稳健性方面进行了验证。所有检测参数均符合生物分析方法验证的当前建议。该方法适用于活性化合物（雷尼替丁）和防腐剂（MP和PP）的常规分析（测定和稳定性试验）。
