HPLC测定匹可硫酸钠的有关物质.docx

目录摘 要3Abstract3引言31. 仪器与试剂41.1仪器41.2试剂42. 检测方法52.1 色谱条件52.2测定方法52.2.1供试品溶液配制52.2.2 样品的测定52.3 实验结果53. 方法学验证63.1方法专属性63.1.1目的63.1.2操作方法63.1.3可接受标准63.1.4方法专属性测试结果63.1.5样品图谱如下63.2系统适应性实验83.2.1目的83.2.2 操作方法83.2.3可接受标准83.2.4 实验结果83.3检测限测试93.3.1目的93.3.2操作方法93.3.3可接受标准93.3.4 实验结果93.4最小定量限测试93.4.1目的93.4.2操作方法93.4.3可接受标准93.4.4实验结果93.5验证范围的线性103.5.1目的103.5.2操作方法103.5.3可接受标准103.5.4 线性数据103.6验证范围内的方法精密度113.6.1目的113.6.2操作方法113.6.3可接受标准113.6.4方法精密度测试数据114.讨论124.1 检测波长的确定124.2 色谱柱的选择124.3 流动相的选择125.结论12参考文献13致 谢14HPLC法检测匹可硫酸钠的有关物质摘 要 目的：确保匹可硫酸钠有关物质检测方法准确、重现并耐用，为建立检验操作程序提供依据。方法：采用高效液相色谱法( HPLC)测定匹克硫酸钠有关物质，以Boston C18柱(250mm×4.6mm，5μm）作为分析色谱柱，以乙腈为流动相A,以0.067 mol·L-1磷酸盐溶液（用NaOH调PH值至7.0）为流动相B;流速为1.0mL·min-1，进样量20μL，检测波长为263nm，柱温30℃。结果：该方法重复性较好，精密度高，匹可硫酸钠有关物质4，4-（2-吡啶亚甲基）双酚浓度在0.03588μg·mL-1 ～294μg·mL-1范围内线性良好（r=0.9995）。结论：本文所建立的高效液相色谱法检测匹可硫酸钠有关物质，方法简捷、省时，结果准确可靠，可成为匹可硫酸钠更科学的的质量控制依据。关键词 匹可硫酸钠; 高效液相色谱法；有关物质；4，4-（2-吡啶亚甲基）双酚钠A HPLC method for determination of the related substances in sodium picosulfateAbstract: Objective：to ensure that the method for determination of the related substances in sodium picosulfate accurate , reproduce and durable , the thesis provides the basis for the establishment of the inspection procedure. Methods: HPLC method was adopted for determination of the related substances in sodium picosulfate, using Agilent C18 columm（250mm×4.6mm，5μm）as the analytical column, the mobile phase A was acetonitrile , and the mobile phase B was phosphate solution(the solution was adjusted by sodium hydroxide solution to PH 7.0), the flow rate was 1.0 ml·min-1，the volume of injection was 20μL，the detection wavelength was 263nm, and the temperature of the column was 30℃. Results: The calibration curve of the related substance named 4,4-[(Pyridin-2-yl)methylene]bisphenol in sodium picosulfate was linear in the range of0.03588 ～294μg·mL-1 (r=0.9995) , the method has a good repeatability and high precision , RSD%=0.500%(n=6). Conclusion:The method for determination of the related s