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目的:建立蜈蚣药材的定性定量分析方法。方法:采用薄层色谱法对蜈蚣药材进行定性鉴别,以三氯甲烷-甲醇-甲酸(10∶1∶1)为展开剂,在紫外光灯(254 nm)下检视;运用高效液相色谱法测定3,8-二羟基喹啉的含量,采用Kromasil C_(18)(250 mm×4.6 mm,5μm)色谱柱,流动相为甲醇-10 mmol·L~(-1)的磷酸二氢钾溶液(32∶68),流速0.8 m L·min~(-1),检测波长252 nm,柱温40℃。结果:薄层鉴别斑点清晰,分离度良好;含量测定中,3,8-二羟基喹啉的线性范围为0.036 2~0.289 6μg(r=0.999 4),平均加样回收率为99.2%(RSD=1.4%,n=6),17批样品中3,8-二羟基喹啉的含量范围为0.175~2.28 mg·g~(-1)。结论:本文建立的薄层色谱鉴别及高效液相色谱含量测定方法可用于蜈蚣药材的质量控制。
Objective: To establish a qualitative and quantitative analysis of centipede herbs. Methods: The centipede medicinal materials were identified by thin-layer chromatography (TLC) with chloroform-methanol-formic acid (10:1:1) as developing solvent and UV light (254 nm). High performance liquid chromatography The content of 3,8-dihydroxyquinoline was determined by using Kromasil C18 (250 mm × 4.6 mm, 5 μm) column. The mobile phase consisted of methanol-10 mmol·L -1 potassium dihydrogen phosphate solution (32:68). The flow rate was 0.8 m L · min -1. The detection wavelength was set at 252 nm and the column temperature was 40 ℃. Results: The identification spots were clear and the separation was good. The linear range of 3,8-dihydroxyquinoline was 0.036 2-0.2889 6μg (r = 0.999 4) and the average recovery was 99.2% (RSD = 1.4%, n = 6). The content of 3,8-dihydroxyquinoline in 17 batches of samples ranged from 0.175 to 2.28 mg · g -1. Conclusion: The TLC and HPLC method established in this paper can be used for the quality control of centipede medicinal materials.