Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, University of Alexandria, Alexandria 21521, Egypt.
Talanta. 2010 Jun 30;82(1):184-95. doi: 10.1016/j.talanta.2010.04.017. Epub 2010 Apr 24.
A simple, rapid and sensitive reversed phase high performance liquid chromatographic method using photodiode array detection was developed and validated for the simultaneous determination of granisetron hydrochloride, benzyl alcohol, 1-methyl-1H-indazole-3-carboxylic acid (the main degradation product of granisetron) and benzaldehyde (the main degradation product of benzyl alcohol) in granisetron injections. The separation was achieved on Hypersil BDS C8 (250 mm x 4.6 mm i.d., 5 microm particle diameter) column using a mobile phase consisted of acetonitrile:0.05 M KH(2)PO(4):triethylamine (22:100:0.15) adjusted to pH 4.8. The column was maintained at 25 degrees C and 20 microL of solutions was injected. Photodiode array detector was used to test the peak purity and the chromatograms were extracted at 210 nm. Naphazoline hydrochloride was used as internal standard. The method was validated with respect to specificity, linearity, accuracy, precision, limit of quantitation and limit of detection. The validation acceptance criteria were met in all cases. Identification of the pure peaks was carried out using library match programmer and wavelengths of derivative optima of the spectrograms of the peaks. The method was successfully applied to the determination of the investigated drugs and their degradation products in different batches of granisetron injections. The method was proved to be sensitive for the determination down to 0.03 and 0.01% of granisetron degradation product and benzaldehyde, respectively, which are far below the compendia limits for testing these degradation products in their corresponding intact drugs.
建立并验证了一种简单、快速和灵敏的反相高效液相色谱法，采用光电二极管阵列检测，用于同时测定盐酸格拉司琼注射液中盐酸格拉司琼、苯甲醇、1-甲基-1H-吲唑-3-羧酸（格拉司琼的主要降解产物）和苯甲醛（苯甲醇的主要降解产物）的含量。在 Hypersil BDS C8（250mm×4.6mmID，5μm 粒径）柱上，以乙腈：0.05M KH（2）PO（4）：三乙胺（22：100：0.15）为流动相，用磷酸调 pH 值至 4.8，实现分离。柱温为 25℃，进样量为 20μL。采用光电二极管阵列检测器检测峰纯度，色谱图在 210nm 处提取。盐酸萘甲唑啉用作内标。该方法经过专属性、线性、准确性、精密度、定量限和检测限验证。所有情况下均符合验证接受标准。采用谱库匹配程序和峰的光谱导数最优波长对纯峰进行鉴定。该方法成功应用于不同批次盐酸格拉司琼注射液中考察药物及其降解产物的测定。该方法对格拉司琼降解产物和苯甲醛的检测灵敏度分别达到 0.03%和 0.01%，远低于相应完整药物中测试这些降解产物的典则限量。
