都梁软胶囊和滴丸中川芎和白芷的鉴别和含量测定方法研究

目的:建立都梁软胶囊、都梁滴丸中川芎和白芷的薄层色谱鉴别方法;建立2种制剂中欧前胡素和异欧前胡素的高效液相色谱含量测定方法。方法:采用正己烷-乙酸乙酯(8:2)为展开剂,以川芎和白芷为对照药材,在紫外光灯(365 nm)下检视;采用Phenomenex Luna C₁₈(2)(250 mm×4.6 mm,5 μm)色谱柱,以乙腈-水(50:50)为流动相,流速1.0 mL·min^-1,检测波长249 nm,柱温25 ℃。结果:川芎和白芷在同一展开系统下薄层色谱主斑点清晰,分离良好。欧前胡素进样量在0.01~0.21 μg(r=0.999 5)范围线性关系良好,异欧前胡素进样量在0.02~0.41 μg(r=0.999 9)范围线性关系良好;都梁软胶囊中欧前胡素和异欧前胡素平均回收率(n=6)分别为99.9%和101.7%,都梁滴丸中欧前胡素和异欧前胡素平均回收率(n=6)分别为98.7%和96.5%。结论:建立的薄层色谱和高效液相色谱方法专属性强,准确度高,重复性好,可用于都梁软胶囊和都梁滴丸的质量控制。

Objective:To develop a TLC method for identification of Chuanxiong Rhizoma and Angelicae Dahuricae Radix in Duliang soft capsules and Duliang dropping pills, and establish an HPLC method for determination of imperatorin and isoimperatorin in above 2 preparations.Methods: An expansion agent system of hexane-ethyl acetate(8:2)was adoped for identification of Chuanxiong Rhizoma and Angelicae Dahuricae Radix.The analysis was performed on a Phenomenex Luna C₁₈ column(250 mm×4.6 mm,5 μm)with the mobile phase of acetonitrile-water(50:50)at a flow rate of 1.0 mL·min^-1.The detection wavelength was set at 249 nm and the column temperature was controlled at 25 ℃.Results:Main spots of Duliang soft capsules and Duliang dropping pills in TLC were clear which a good exhibited separation was observed.A good linearity was obtained with imperatorin in the range of 0.01-0.21 μg(r=0.999 5)and isoimperatorin in the range of 0.02-0.41 μg(r=0.999 9); the average recovery of imperatorin was 99.9%(n=6)and the average recovery of isoimperatorin was 101.7%(n=6)in Duliang soft capsules; the average recovery of imperatorin was 98.7%(n=6)and the average recovery of isoimperatorin was 96.5%(n=6)in Duliang dropping pills.Conclusion: The established method is specific, accurate and reproducible, which can be used for quality control of the Duliang soft capsules and Duliang dropping pills.