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

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。

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×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.