车前子中车前素的TLC鉴别及HPLC含量测定

目的: 建立车前子中车前素的薄层色谱鉴别及高效液相色谱含量测定的方法。方法: 采用薄层色谱法对车前素进行定性鉴别,以乙酸乙酯-甲醇-甲酸(10: 0.5: 2)为展开剂,以碘化铋钾-碘化钾碘(1: 1)试液为显色剂;并采用高效液相色谱法测定车前素的含量,使用CAPCELL PAK C₁₈ MG Ⅱ S5(250 mm× 4.6 mm,5 μm)色谱柱,以乙腈-水(8: 92)为流动相,流速1.0 mL·min^-1,检测波长210 nm,柱温30 ℃。结果: 薄层色谱法能鉴别检出车前素。车前素在进样量0.036 24~0.724 8 μg范围内与峰面积呈现良好的线性关系(r=0.999 9);平均回收率(n=6)为102.5%,RSD为0.84%;15批样品中车前素含量为0.698~3.695 mg·g^-1。结论: 4批生品车前子及由其炮制成的盐炙车前子的车前素含量未见明显差异,10个产地的11批生品车前子中车前素含量有一定差异;该方法分离效率高,重复性好,可作为实验室方法改进的参考依据,为车前子的质量标准的提升做准备。

Objective: To establish the methods for the identification and determination of plantagoguanidinic acid in Plantaginis Semen by TLC and HPLC. Methods: Plantagoguanidinic acid was identified by TLC,using ethyl acetate-methanol-formic acid (10: 0.5: 2)as the mobile phase and bismuth potassium iodide-potassium iodide iodine (1: 1)as the chromogenic agent;and the content of plantagoguanidinic acid was detected by HPLC.The separation was carried out on a CAPCELL PAK C₁₈ MG Ⅱ S5 (250 mm×4.6 mm,5 μm)column with the mobile phase of acetonitrile-water (8: 92);the flow rate was 1.0 mL·min^-1;the detection wavelength was 210 nm;the column temperature was at 30 ℃. Results: Plantagoguanidinic acid could be identified by TLC.The linear range of plantagoguanidinic acid was 0.036 24-0.724 8 μg (r=0.999 9),the average recovery was 102.5%,and RSD was 0.84%.The content of plantagoguanidinic acid in 15 samples was 0.698-3.695 mg·g^-1. Conclusion: There were no obvious differences between the 4 raw products and the salt products which were prepared from the raw products of plantagoguanidinic acid in Plantaginis Semen,and there were certain differences in contents of plantagoguanidinic acid in 11 batches of raw Plantaginis Semen from 10 different habitats.This method with high separation efficiency and good repeatability can be used as a reference for improvement of laboratory methods and the preparation for improvement of the quality standard of Plantaginis Semen.