HPLC同时测定补肾活血颗粒中松脂醇二葡萄糖苷、苦杏仁苷、桂皮醛的含量

Simultaneous Determination of Pinoresinol Diglucoside, Amygdalin and Cinnamylaldehyde in Bushen Huoxue Granule

目的 采用HPLC波长切换法,建立同时测定补肾活血颗粒中松脂醇二葡萄糖苷、苦杏仁苷、桂皮醛3成分含量的分析方法。方法 采用Zorbax Extend-C18柱（4.6 mm×150 mm,5μm）;以乙腈-水为流动相梯度洗脱,松脂醇二葡萄糖苷、苦杏仁苷、桂皮醛的检测波长分别为227,210,290 nm;进行样品前处理工艺和方法学考察。结果 松脂醇二葡萄糖苷、苦杏仁苷和桂皮醛均得到很好分离,浓度分别在0.426 0~2.88 6μg.mL1,7.455~86.60μg.mL1和0.440 6~13.22μg.mL1内线性关系良好（r≥0.999）;平均加样回收率分别为98.3%（RSD=1.6%）,101.4%（RSD=1.1%）和100.0%（RSD=1.2%）;精密度试验峰面积RSD均≤1.4%。结论 该方法预处理简单,方法灵敏、准确、重复性好,可用于补肾活血颗粒及相关制剂的质量控制。

OBJECTIVE To establish an HPLC method for determination of pinoresinol diglucoside, amygdalin, and cinnamylaldehyde in Bushen Huoxue granule. METHODS Agilent Zorbax Extend-C18（4.6 mm×150 mm, 5 μm） was adopted; the mobile phase was acetonitrile-water with gradient elution at a flow rate of 1.0 m L·min？1, and the detection wavelength was 210 nm（0？5 min） for amygdalin, 227 nm（5？10 min） for pinoresinol diglucoside, 290 nm（10？14 min） for cinnamylaldehyde. The methodological study included sample pre-treatment process and method validation. RESULTS The components of pinoresinol diglucoside, amygdalin, and cinnamylaldehyde were well separated, the method had a good linearity in the range of 0.426 0？ 2.88 6 μg·m L？1, 7.455？86.60 μg·m L？1 and 0.440 6？13.22 μg·m L？1（r≥ 0.999）; the average recoveries were 98.3%（RSD=1.6%）, 101.4%（RSD=1.1%）, 100.0%（RSD=1.2%）, respectively, and the RSDs of intra-day and inter-day assays were all ≤1.4%. CONCLUSION This method was simple, sensitive and reproducible and can be used for the quality control of Bushen Huoxue granule and its related preparation.