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

关键词:  补肾活血颗粒  高效液相色谱法  波长切换法  含量测定

Key words:  Bushen Huoxue granule  HPLC  wavelength switching  content determination

摘要:

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，5 μm)；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 6 μg?mL^-1，7.455~86.60 μg?mL^-1和0.440 6~13.22 μg?mL^-1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。

Abstract:

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 mL?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?mL^-1 7.455-86.60 μg?mL^-1and 0.440 6?13.22 μg?mL^-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.