色谱

色谱 ›› 2010, Vol. 28 ›› Issue (08): 805-808.DOI: 10.3724/SP.J.1123.2010.00805

• 技术与应用 • 上一篇    下一篇

超高效液相色谱法测定青娥丸中松脂醇二葡萄糖苷的含量

张紫佳1,2, 陈洁1,2, 赵骏铭1,2, 廖立平1,2, 孙庆龙3, 吴弢1,2*, 王峥涛1,2   

  1. 1. 上海中医药大学中药研究所, 中药标准化教育部重点实验室, 中药新资源与质量标准综合评价国家中医药管理局重点研究室, 上海 201210; 2. 上海中药标准化研究中心, 上海 201210; 3. 沃特世科技（上海）有限公司, 上海 200233
  • 收稿日期:2010-03-18 修回日期:2010-05-27 出版日期:2010-08-28 发布日期:2010-08-28
  • 通讯作者: 吴弢,博士,研究员,研究方向为中药的活性成分与质量标准.
  • 基金资助:

    国家自然科学基金项目(编号: 30901952)、教育部高等学校科技创新工程重大项目培育资金项目(编号: 706025)、国家药典委员会项目(ZH-398)和上海市教委高校创新团队建设经费资助项目.

10.3724/SP.J.1123.2010.00805

ZHANG Zijia1,2, CHEN Jie1,2, ZHAO Junming1,2, LIAO Liping1,2, SUN Qinglong3, WU Tao1,2*, WANG Zhengtao1,2   

  1. 1. The Ministry of Education (MOE) Key Laboratory for Standardization of Chinese Medicines and The State Administration of Traditional Chinese Medicine (SATCM) Key Laboratory for New Resources and Quality Evaluation of Chinese Medicines, Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai 201210, China; 2. Shanghai R. & D. Center for Standardization of Chinese Medicines, Shanghai 201210, China; 3. Waters Technologies (Shanghai) Limited, Shanghai 200233, China
  • Received:2010-03-18 Revised:2010-05-27 Online:2010-08-28 Published:2010-08-28

PDF

570

被引次数

15

摘要： 建立了超高效液相色谱(UPLC)测定青娥丸中主要活性成分松脂醇二葡萄糖苷(pinoresinol diglucoside, PDG)含量的方法。样品经索氏提取后,提取物再用Waters Oasis HLB SPE固相萃取小柱进行前处理以消除杂质对PDG色谱峰的干扰。色谱条件：采用Waters Acquity C18 BEH UPLC柱(100 mm×1.0 mm, 1.7 μm)分离,以乙腈-水(使用磷酸调pH值至4.0)(9:91, v/v)为流动相,流速为0.1 mL/min,检测波长为227 nm,柱温为25 ℃,进样量为0.5 μL。在上述条件下,松脂醇二葡萄糖苷在1.40～506.00 mg/L范围内呈现良好的线性关系,相关系数r=1;低、中、高3个添加水平下的平均回收率分别为100.51%、102.37%、100.10%(n=9)。该方法准确、灵敏、重现性好,可用于青娥丸的质量控制。

关键词: 超高效液相色谱, 青娥丸, 松脂醇二葡萄糖苷

Abstract: A new ultra performance liquid chromatographic (UPLC) method was established for the determination of pinoresinol diglucoside (PDG) in Qing’e Pills. After extracted by the Soxhlet’s method, the methanol extracts of the samples were passed through a Waters Oasis HLB SPE column to achieve good chromatographic performance. The separation was performed on a Waters Acquity C18 BEH column (100 mm×1.0 mm, 1.7 μm) with acetonitrile-water (the pH adjusted to 4.0 with phosphoric acid) (9:91, v/v) as the mobile phase at a flow rate of 0.1 mL/min. The detection wavelength was set at 227 nm, the column temperature was 25 ℃ and the injection volume was 0.5 μL. Under the optimized conditions, there was good linear relationship between the mass concentration and the peak area of PDG in the range of 1.40-506.00 mg/L with the correlation coefficient of 1. The average recoveries of PDG at three levels ranged from 100.10% to 102.37%. The method is accurate, sensitive, highly reproducible and suitable for the quality control of Qing’e Pills.

Key words: pinoresinol diglucoside, Qing’e Pill, ultra performance liquid chromatography (UPLC)