RP-HPLC测定去甲斑蝥素含量及有关物质  

Determination of Norcantharidin and Its Related Substances by HPLC

作　　者：李春民[1] 赵桂森[1] 袁玉梅[1] 

机构地区：[1]山东大学药学院药物化学研究所,济南250012

出　　处：《中国药学杂志》2007年第6期469-472,共4页Chinese Pharmaceutical Journal

基　　金：国家自然科学基金(20472045;20672069);山东省自然科学基金(Y2003C19)

摘　　要：目的建立去甲斑蝥素原料药含量及有关物质的反相高效液相色谱测定方法。方法色谱柱为YWG-C18（4．6mm×250mm，5μm），流动相为甲醇-0．016mol·L^-1磷酸二氢钾溶液（30：70）（用磷酸调节pH值至3．1），检测波长为213nm，流速为0．9mL·min^-1。结果去甲斑蝥素与马来酸酐、去氢去甲斑蝥素及其降解产物均能较好的分离，且线性良好（r分别为0．9998，0．9999，0．9997）；检测下限分别为10．0，0．08，0．63ng（S／N=3），平均回收率（n=9）分别为99．94％，100．43％，100．03％；含量测定方法的线性范围为0．126-4.044g·L^-1。结论方法简便，结果准确，重复性好，适用于该产品含量及有关物质测定。OBJECTIVE To develop a RP-HPLC method for the determination of norcanthafidin and its related substances, METHODS A chromatography was carried out on a YWG -C18 column （4.6 mm × 250 mm, 5 μm） , using a mobile phase consisting of methanol -0, 016 mol·L^-1 potassium dihydrogen phosphate （30： 70） （adjusted to pH 3.1 with phosphoric acid）. The detection was carried out with a UV detector at 213 nm, The flow rate was 0. 9 mL·min^-1. RESULTS Norcantharidin, maelic anhydride, dehydronorcantharidin and degradation products were separated. The calibration curves of norcantharidin, maelic anhydride and dehydronorcantharidin were linear （r = 0. 999 8,0. 999 9,0. 999 7）. The detection limits were 10.0 ng for norcantharidin, 0. 08 ng for maelic anhydride and 0. 63 ng for dehydronorcantharidin, respectively （ S/N = 3 ）. The recoveries of norcantharidin, maelic anhydride and dehydronorcantharidin were 99. 94%, 100. 43% and 100. 03%, respectively（ n = 9）. The norcantharidin curves were linear in the range of 0. 126 -4. 044 g·L^-1. CONCLUSION This method is convenient, accurate and suitable for the determination of norcantharidin and related substances.

关 键 词：反相高效液相色谱法 去甲斑蝥素 有关物质 

分 类 号：R917[医药卫生—药物分析学]