氯法拉滨质检及评价.pdfVIP

氯法拉滨质检及评价 摘 要 本文是采用高效液相色谱法对注射用氯法拉滨进行质量分析的测定，旨在建立 一种简单、快捷和灵敏的检测有关物质和含量的色谱分析方法。在本实验中采用岛 津 LC-20AT 泵、SPD-20AVP 紫外检测，流动相为磷酸盐缓冲液（磷酸氢二钾 6.8g 于 1000ml 量瓶中，加水适量，调节 pH 到 3.0 ±0.05 ）：乙腈=88 ：12，色谱柱为 YMC-C18, 5µm, 4.6×150mm ，检测波长为 265nm，流速为 1.0ml/min，进样量为 20µl ， 柱温为 25 ℃，检测限为4ng ，定量限为 12ng。采用上述色谱条件对样品进行破坏 性试验，本品在各条件下的降解产物与主峰分离良好，以混合溶液（流动相 A ：流 动相 B=90:10 ）溶解并稀释，发现氯法拉滨在0.1～1.6µg 范围内与其峰面积呈良好 的线性关系。相关系数r 为 0.9999，相关系数良好，测定注射用氯法拉滨的回收率 和重复性良好，在室温条件下 8 小时内稳定，因此可在室温条件下放置。实验结果 显示在上述条件下对氯法拉滨进行色谱分析的方法是快速，准确和可行的。 关键词：氯法拉滨，高效液相，含量测定 I 氯法拉滨质检及评价 Abstract This paper is used for high-performance liquid chromatography injection clofarabine quality of the determination to establish a simple, fast and sensitive detection of the material and content of the chromatographic analysis. In this experiment in the use of Shimadzu LC-20AT pump, SPD-20AVP UV detection, mobile phase of phosphate buffer (K2HPO4 6.8 g in 1000 ml Liangping, adequate water, adjusting the pH to 3.0 ± 0.05 ): = 88:12 acetonitrile, the column for the YMC-C18, 5 μ m, 4.6 × 150mm, detection at 265 nm, a flow rate of 1.0 ml / min, sample volume for the 20 μ l, temperature for 25 ℃, for the detection limit 4ng, quantitative limit of 12 ng. By using the above conditions on samples of destructive testing, in all the goods under the condition of degradation products from the main peak and the good, a mixed solution (mobile phase A: mobile phase B = 90:10) dissolved and diluted, found clofarabine In the 0.1 ~ 1.6 μ g within the framework of its peak area was a good linear relationship. The correlation coefficient r 0.9999, good correlation