璇玑化痞膏-中国药品标准.docVIP

银杏叶提取物中槐角苷检查方法的研究 刘颖1,2 ，宋彬彬1，付龙1，1,2，钱忠直1,3* ChP-Waters联合开放实验室，北京100061 北京市药品检验所，北京 1022063.国家药典委员会，北京 100061） 摘要对银杏叶提取物中槐角苷检方法研究。超高效液相高效液相结果高效液相色谱在2.～43.9ng范围内呈良好的线性关系（r＝1.000 0），加样回收率为101.5%，RSD为2.1%；超高效液相色谱在0. 4～6.5ng范围内呈良好的线性关系（r=0.999 9），加样回收率为104.0%，RSD为1.6%。结论所建方法前处理简便易行，采用超高效液相色谱法测定迅速，节能环保，适合于应急快速检验；采用高效液相色谱法通用性好，适合检验；两种方法均有很好的重复性，可银杏叶提取物中槐角苷的补充检方法。 关键词：银杏叶提取物；槐角苷；；；光电二极管阵列检测器 Study on Detection Method for Sophoricoside in Ginkgo LeavesExtract Liu Ying1,2, Song Binbin1, Fu Long1, Gao Qing1,2, Qian Zhongzhi1,3* (1.ChP-Waters Joint Open Laboratory, Beijing 100061；2. Beijing Institute for Drug Control, Beijing 102206； 3.Chinese Pharmacopeia Commission, Beijing 100061) Abstract Objective: To establish a detection method for Sophoricoside in Ginkgo Leaves Extract. MethodsThe content of Sophoricoside was determined by UPLC and HPLC. An ACQUITY UPLC BEH Shield RP18 column（ 2.1mm×100mm，1.7μm）and a Shield RP18 column（4.6mm×250mm，5μm）were adopted for UPLC and HPLC , respectively. Acetonitrile was mobile phase A and 0.1% phosphoric acid was mobile phase B, gradient elution. The column was set at 30℃and the detection wavelength was 260nm. Results: In HPLC, Sophoricoside showed good linear realationship in the range of 2.2–43.9ng (r=1.000 0), the average recovery was 101.5%with RSD of 2.1 %. In UPLC, the good linear relationship showed in the range of 0. 40–6.5ng (r=0.999 9), the average recovery was 104.0%withRSD of 1.6 %. Conclusion: The UPLC method provides high speed with reduced solvent consumption, which is suitable for emergency rapid test. HPLC method is commonly used and can be adopted by most laboratories. Both methods are easy to process, reproducible, and can be used as supplemental method for Sophoricoside detection in Ginkgo Leaves Extract. Key words： Ginkgo Leaves Extract; Sophoricoside; UPLC; HPLC; PAD 银杏叶提取物的质量在2015年受到了社会的普遍关注，国家食品药品监督管理总局在对银杏叶制剂原料药生产企业的飞行检查中，发现个别生产企业不仅有擅自修改提取工艺的现象，而且有银杏叶提取的迹象。为更好控制银杏叶提取物的内在质量，对槐角苷超高效液相色谱（UPLC）高效液相色谱（HPLC）的检方法，并对该方法