Breuzovska Katerina, Dimitrovska Aneta, Kitanovski Zoran, Petrusevska Jelena, Ribarska Jasmina Tonic, Jolevska Suzana Trajkovic
University Ss. Cyril and Methodius, Center for Drug Quality Control, Faculty of Pharmacy, Vodnjanska 17, Skopje, Macedonia.
J AOAC Int. 2010 Jul-Aug;93(4):1113-20.
A method based on RP-HPLC with indirect UV detection was developed for the determination of phosphates and phosphites as impurities in sodium risedronate. RP separation of the phosphates and phosphites was achieved by adding tetrabutylammonium hydroxide as an ion-pairing agent in the mobile phase. Potassium hydrogen phthalate was added to the mobile phase as an ionic chromophore in order to obtain high background absorption of the mobile phase. Separation was performed on a C18 column using a mixture of pH 8.2 buffer (containing 0.5 mM tetrabutylammonium hydroxide and 1 mM phthalate) and acetonitrile (95 + 5, v/v) as the mobile phase, with indirect UV detection at 248 nm. The validation of the method included determination of specificity/selectivity, linearity, LOD, LOQ, accuracy, precision, and robustness. The LOD was 0.86 microg/mL for phosphates and 0.76 microg/mL for phosphites. The LOQ was 2.60 microg/mL for phosphates and 2.29 microg/mL for phosphites. The developed method is suitable for quantitative determination of phosphates and phosphites as impurities in QC of sodium risedronate.
建立了一种基于反相高效液相色谱（RP-HPLC）间接紫外检测法，用于测定利塞膦酸钠中作为杂质的磷酸盐和亚磷酸盐。通过在流动相中加入氢氧化四丁铵作为离子对试剂，实现了磷酸盐和亚磷酸盐的RP分离。向流动相中加入邻苯二甲酸氢钾作为离子发色团，以获得流动相的高背景吸收。在C18柱上进行分离，使用pH 8.2缓冲液（含有0.5 mM氢氧化四丁铵和1 mM邻苯二甲酸盐）和乙腈（95 + 5，v/v）的混合物作为流动相，在248 nm处进行间接紫外检测。该方法的验证包括特异性/选择性、线性、检测限（LOD）、定量限（LOQ）、准确度、精密度和稳健性的测定。磷酸盐的LOD为0.86 μg/mL，亚磷酸盐的LOD为0.76 μg/mL。磷酸盐的LOQ为2.60 μg/mL，亚磷酸盐的LOQ为2.29 μg/mL。所建立的方法适用于利塞膦酸钠质量控制中作为杂质的磷酸盐和亚磷酸盐的定量测定。
