目的: 建立高效液相色谱法同时测定不同产地的高良姜药材中原儿茶酸、槲皮素、山柰酚、高良姜素、姜黄素和大黄素含量。 方法: 采用Phenomenex C18色谱柱(250 mm×4.6 mm,5 μm),以0.1%醋酸溶液(A)-乙腈(B)为流动相,梯度洗脱(0~5 min,35%B→60%B;5~10 min,60%B;10~15 min,60%B→35%B),流速0.8 mL·min-1,检测波长260 nm,柱温35 ℃。 结果: 原儿茶酸、槲皮素、山柰酚、高良姜素、姜黄素和大黄素浓度分别在0.0287~143.33 μg·mL-1(r=0.9997)、0.0267~133.33 μg·mL-1(r=0.9999)、0.0233~116.67 μg·mL-1(r=0.9999)、0.022~110.00 μg·mL-1(r=0.9997)、0.034~170.00 μg·mL-1(r=0.9998)、0.0207~103.33 μg·mL-1(r=0.9996)范围内与峰面积呈良好的线性关系,平均加标回收率(n=9)均在93.07%~98.77%范围内,仪器精密度(n=6)的RSD均小于3.8%,方法重复性(n=6)的RSD均小于3.1%。 结论: 该分析方法经方法学验证,可作为高良姜中6个成分的检测方法。
Objective: To develop an HPLC method for simultaneous determination of 3,4-dihydroxybenzonic acid,quercetin,kaempferol,galangin,curcumin and emodin in Alpinia officinarum. Methods: The HPLC system consisting of a C18 column(250 mm×4.6 mm,5 μm) and a mixture of 0.1% acetic acid (A)-acetonitrile (B) with gradient elution (0-5 min,35%B→60%B;5-10 min,60%B;10-15 min,60%B→35%B) as the mobile phase was adopted,and the flow rate was 0.8 mL·min-1.The UV detective wavelength was 260 nm,and the column temperature was set at 35 ℃. Results: The linear response ranged from 0.0287-143.33 μg·mL-1 for 3,4-dihydroxybenzonic acid(r=0.9997),0.0267-133.33 μg·mL-1 for quercetin(r=0.9999),0.0233-116.67 μg·mL-1 for kaempferol (r=0.9999),0.022-110.00 μg·mL-1 for galangin(r=0.9997),0.034-170.00 μg·mL-1 for curcumin(r=0.9998),and 0.0207-103.33 μg·mL-1 for emodin (r=0.9996),respectively.The recoveries (n=9) of six active components were 93.07%-98.77%.All of the RSD of precision(n=6) and repeatability (n=6) were below 3.8% and 3.1%. Conclusion: The validation data demonstrated that the method could be used to measure the six flavonoids in Alpinia officinarum.