[关键词]
[摘要]
目的 建立桂附地黄丸中马钱苷、芍药苷、丹皮酚和没食子酸含量同时测定的高效液相色谱法。方法 采用Phenmenex Synergri Fusion RP 80A色谱柱(250 nm × 4.6 nm,4 μm);流动相为乙腈-0.05 %磷酸溶液,梯度洗脱,体积流量为1 mL·min-1,检测波长为234 nm和274 nm,柱温为30 ℃。结果 马钱苷、芍药苷、丹皮酚和没食子酸的线性范围分别为5.3408 ~ 48.0672 μg·mL-1(r=0.9999),4.8256~43.4303 μg·mL-1(r=0.9996),10.8134~97.3206 μg·mL-1(r=0.9999),4.1240~37.116 μg·mL-1(r=0.9999)。平均加样回收率分别为马钱苷100.7 %,RSD=0.85 %(n=6);芍药苷101.1 %,RSD=1.98 %(n=6);丹皮酚98.9 %,RSD=0.55 %(n=6);没食子酸99.8 %,RSD=1.25 %(n=6)。结论 该方法操作简便、准确,重复性好,可用于桂附地黄丸的质量控制。
[Key word]
[Abstract]
Objective To develop a simple high performance liquid chromatography(HPLC) method for the determination of loganin,paeoniflorin, paeonol and gallic acid in Guifu Dihuang pills. Methods The HPLC method was validated on Phenmenex Synergri Fusion-RP column(250 nm × 4.6 nm,4 μm) with a mobile phase of acetonitrile-0.05 % phosphoric acid at a flow rate of 1 mL/min and a column temperature of 30 ℃. The detection wavelengths were set at 234 nm and 274 nm.Results The calibration curve of the loganin,paeoniflorin,paeonol and gallic acid showed good linearity relationship in the range of 5.3408 ~ 48.0672 μg·mL-1(r=0. 9999),4.8256 ~ 43.4303 μg·mL-1(r=0.9996),10.8134 ~ 97.3206 μg·mL-1(r=0.9999),4.1240~37.1160 μg·mL-1(r=0.9999),respectively. The average recovery was 100.7 % for loganin,101.1 % for paeoniflorin,98.9 % for paeonol and 99.8 % for gallic acid,and the standard deviations were 0.85 %,1.98 %,0.55 % and 1.25 %,respectively(n=6). Conclusion The developed method is simple and rapid with excellent specificity,accuracy and precision,which can be used for the quality control of Guifu Dihuang Pills.
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[基金项目]
广东省211工程三期重点学科建设项目[粤发改社(2009)972号];广东省自然科学基金(9451040701002867)。