Zhang Zijia, Chen Jie, Zhao Junming, Liao Liping, Sun Qinglong, Wu Tao, Wang Zhengtao
The Ministry of Education (MOE) Key Laboratory for Standardization of Chinese Medicines, Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai 201210, China.
Se Pu. 2010 Aug;28(8):805-8. doi: 10.3724/sp.j.1123.2010.00805.
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 x 1.0 mm, 1.7 microm) 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 degrees C and the injection volume was 0.5 microL. 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.
建立了一种新的超高效液相色谱（UPLC）法测定青娥丸中松脂醇二葡萄糖苷（PDG）的含量。样品经索氏提取法提取后，甲醇提取物通过Waters Oasis HLB固相萃取柱以获得良好的色谱性能。采用Waters Acquity C18 BEH柱（100 mm×1.0 mm，1.7μm）进行分离，以乙腈-水（用磷酸调pH至4.0）（9:91，v/v）为流动相，流速为0.1 mL/min。检测波长设定为227 nm，柱温为25℃，进样量为0.5μL。在优化条件下，PDG质量浓度在1.40 - 506.00 mg/L范围内与峰面积具有良好的线性关系，相关系数为1。PDG在三个水平的平均回收率为100.10%至102.37%。该方法准确、灵敏、重现性高，适用于青娥丸的质量控制。
