表2专属性试验主峰的峰纯度.PDFVIP

·药物分析与检验 · HPLC 测定二-(2,4-二氟苯甲酰异羟肟酸)二苯基合锡原料药的含量及 有关物质 高竹妍，郑娟，李云兰* ，李青山( 山西医科大学药学院，太原 030001) 摘要：目的 建立反相高效液相色谱法测定有机锡类抗癌化合物二-(2,4-二氟苯甲酰异羟肟酸)二苯基合锡(DPDFT)原料药 的含量及有关物质。方法 分析柱为 Diamonsil C18 (250 mm×4.6 mm ，5 µm) ；以甲醇-水(20 ∶80 ，用磷酸调 pH 至 3.0)为 流动相；流速为 0.8 mL·min1 ；含量测定检测波长为 228 nm ，有关物质检测波长为 246 nm ，柱温为 25 ℃。结果 样品 7 中待测组分与有关物质分离良好，平均回收率为 99.0% ，RSD 为 0.65%(n=9) ，回归方程为 A=1.65×10 C3 286 (r=0.999 9) ， 1。最低检测限为 10 ng。结论 本方法操作简便快速，结果准确，专属性强，灵敏度高，可同 线性范围为 1.7~150 µg·mL 时用于抗癌化合物 DPDCT 原料药的含量控制及有关物质检查。 关键词：二-(2,4-二氟苯甲酰异羟肟酸)二苯基合锡；含量测定；有关物质；高效液相色谱法 中图分类号：R917.101; R927.2 文献标志码：B 文章编号：1007-7693(2010)11-1119-03 Determination of Crude Drug Di-phenyl-di-(2,4-difluobenzohydroxamato) tin and Its Related Substances by HPLC * GAO Zhuyan, ZHENG Juan, LI Yunlan , LI Qingshan(School of Pharmaceutical Science, Shanxi Medical University, Taiyuan 030001, China) ABSTRACT: OBJECTIVE To establish a method to determine the content of crude drug di-phenyl-di-(2,4- diflurobenzohydroxamato)tin (DPDFT) and its related substances by RP-HPLC. METHODS The HPLC system was adopted with Diamonsil C18(250 mm× 4.6 mm, 5 µm) as the stationary phase. The mobile phase was consisted of methanol-water (20 ∶80, adjusted to pH 3.0 with phosphoric acid) with the flow rate of 0.8 mL·min1 and column temperature was 25 ℃ . The detection wavelength for determination of contents and related substances were set at 228 nm and 246 nm, respectively. RESULTS Under the selected chromatographic conditions, related substances and degraded substances were completely separated from DPDFT. The