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目的建立益母草中水苏碱、益母草碱含量测定的高效液相色谱法。方法生药经乙酸乙酯脱色后,用乙醇超声提取,得样品。采用YMC-Park CN 柱(250.0 mm×4.6 mm);水苏碱测定用流动相为0.001 25 mol/L SDS(含0.05%高氯酸) ∶乙腈(90∶10),流速1.5 ml/min,检测波长201.7nm;益母草碱测定用流动相为0.001 25 mol/L SDS(含0.05%高氯酸)∶甲醇(50∶50),流速1 ml/min,检测波长282 nm;灵敏度0.1AUFs,柱温20 ℃。外标法定量。结果以进样量( mg )为横坐标,峰面积为纵坐标,水苏碱回归方程为Y=1187.542 3X-168.982 2;益母草碱回归方程为Y=5202.654X-221.141(r=0.9998),线性范围2.5~12.5 mg,最小检出限0.15 mg,加样回收率为(99.030±2.744)%。18个不同地区样品分析结果显示,不同产地的药材中两种生物碱的含量差异甚大,水苏碱约在0.1%~0.2%,益母草碱在生药中含量很低,约在0.01%~0.05%之间。总体而言,产于北方者生物碱含量较高,而产于南方者普遍较低。益母草及其变种白花益母草总生物碱含量在0.3%左右,高于其他品种。结论用高效液相色谱法测定益母草中生物碱含量,简便易行,结果准确可靠,优于以前的方法。
Objective To establish HPLC method for the determination of stachydrine and Leonurine in Motherwort. Methods The crude drug was decolorized with ethyl acetate and extracted with ethanol to obtain samples. The YMC-Park CN column (250.0 mm×4.6 mm) was used; the mobile phase was 0.001 25 mol/L SDS (containing 0.05% perchloric acid):acetonitrile (90:10), and the flow rate was 1.5 ml/min. The detection wavelength was 201.7nm; the mobile phase for the detection of Leonurine was 0.001 25 mol/L SDS (containing 0.05% perchloric acid): methanol (50:50), the flow rate was 1 ml/min, the detection wavelength was 282 nm, and the sensitivity was 0.1AUFs. Temperature 20 °C. External standard method. Results The injection volume (mg) was plotted on the abscissa and the peak area was plotted on the ordinate. The regression equation for stachyose was Y=1187.542 3X-168.982 2. The regression equation for leucovorin was Y=5202.654X-221.141 (r=0.9998). The range is 2.5~12.5 mg, the minimum detection limit is 0.15 mg, and the recovery rate of addition is (99.030±2.744)%. The results of analysis of samples from 18 different regions showed that the contents of two alkaloids in herbs from different habitats vary greatly. Stachydrine is about 0.1% to 0.2%, and leondrozine is low in crude drugs, about 0.01% to 0.05%. between. In general, alkaloids are higher in people born in the North, while those in the North are generally lower. The total alkaloid content of Motherwort and its variant Baihua Leonurus was about 0.3%, which was higher than other varieties. Conclusion Determination of alkaloids in Herba Leonuri by high performance liquid chromatography is simple and accurate. The results are more accurate and reliable than the previous methods.