| 引用本文: | 高竹妍,郑娟,李云兰,李青山.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[J].中国现代应用药学,2010,27(12):1119-1121. |
| .Determination of Crude Drug Di-phenyl-di-(2,4-difluobenzohydroxamato) tin and Its Related Substances by HPLC[J].Chin J Mod Appl Pharm(中国现代应用药学),2010,27(12):1119-1121. |
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| 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=1.65×107C-3 286 (r=0.999 9)，线性范围为1.7~150 µg·mL-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 |
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| Determination of Crude Drug Di-phenyl-di-(2,4-difluobenzohydroxamato) tin and Its Related Substances by HPLC |
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GAO Zhuyan ZHENG Juan LI Yunlan* LI Qingshan
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| 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 average recovery was 99.0 % and the RSD was 0.65%(n=9). The linear range was 1.7-150 µg·mL-1, and the regression equation was A=1.65×107C-3 286 (r=0.999 9). The limit of detection was10 ng. CONCLUSION The analytical method was simple, quick, accurate, sensitive and selective for the determination of crude drug DPDFT and its related substances. |
| Key words: di-phenyl-di-(2,4-diflurobenzohydroxamato)tin content related substances HPLC |
