HPLC法测定2-甲氧基雌二醇原料药中主药和有关物质的含量.pdfVIP

HPLC 法测定2- 甲氧基雌二醇原料药中主药和有关物质的含量 1＊ 2 2 2 2# 李 杨 ，施秀芳 ，王丹丹 ，张超峰 ，杜 斌 （1.河南省食品药品检验所，郑州市 450003；2.郑州大学药学 院，郑州市 450001） + 中图分类号 R927.2；R977.12 文献标识码 A 文章编号 1001-0408（2011）45-4280-03 摘 要 目的：建立测定2- 甲氧基雌二醇原料药中主药及有关物质含量的方法。方法：采用高效液相色谱法。色谱柱为Agilent Eclipse XDB-C18；流动相为甲醇-水（65∶35），流速为1.0mL ·min－1；柱温为30℃；检测波长为285nm 。结果：2- 甲氧基雌二醇与杂 质分离度良好，其检测浓度线性范围为45.96～229.8μg ·mL－1（r ＝0.9998，n ＝5），检测限和定量限分别为2、10ng ；3批样品的有关 物质含量均低于2.0％。结论：该方法准确、快速、分离度好、灵敏度高，可用于2- 甲氧基雌二醇原料药的质量控制。 关键词 高效液相色谱法；2- 甲氧基雌二醇；原料药；含量测定；主药；有关物质 Content Determination of Main Component and Related Substances of 2-Methoxyestradiol by HPLC LI Yang （Henan Provincial Institute for Food and Drug Control ，Zhengzhou 450003，China ） SHI Xiu-fang ，WANG Dan-dan ，ZHANG Chao-feng ，DU Bin （School of Pharmacy ，Zhengzhou University ， Zhengzhou 450001，China ） ABSTRACT OBJECTIVE ：To establish a method for the content determination of 2-methoxyestradiol and its related substances. METHODS ：HPLC method was adopted. Agilent Eclipse XDB-C18 column was adopted with methanol-water （65∶35）as mobile phase at the flow rate of 1.0 mL ·min －1. The detection wavelength was set at 285 nm and column temperature was 30 ℃. RE- SULTS ：Good separation of 2-methoxyestradiol and related substance could be achieved. The standard curve was linear in the range of 45.96－229.8 μg ·mL －1（r ＝0.999 8，n ＝5）．The limit of detection and quantification was 2 ng and 10ng respectively ，and the total contents of the related substances in 3batches samples were all below 2.0％. CONCLUSION ：The method is accurate ，rapid ， well-separated and sensitive ，and it can be used for the quality control of 2-methoxyestradiol. KEY WORDS HPLC ；2-Methoxyestradiol ；Raw material ；Content determination ；Main component ；Related substances 2- 甲氧基雌二醇（2-Methoxyestradiol ，2-ME）为雌二醇的 2-ME 原料药（批