南方医科大学学报

南方医科大学学报 ›› 2004, Vol. 24 ›› Issue (11): 1223-1226.

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反向离子对色谱法测定益母草药材中水苏碱和益母草碱的含量

晁志1, 马丽玲2, 周秀佳3   

  1. 1. 南方医科大学中医系, 广东, 广州, 510515;
    2. 广州卫生学校药检学科组, 广东, 广州, 510020;
    3. 上海中医药大学中药学院, 上海, 200032
  • 出版日期:2004-11-20 发布日期:2004-11-20
  • 基金资助:
    作者简介:Chao Zhi(1971- ),PhD,E-mail:chaozhi1971@yahco.com.cn

Determination of stachydrine and leonurine in Herba Leonuri by ion- pair reversed-phase high-performance liquid chromatography

CHAO Zhi1, MA Li-ling2, ZHOU Xiu-jia3   

  1. 1. 南方医科大学中医系, 广东, 广州, 510515;
    2. 广州卫生学校药检学科组, 广东, 广州, 510020;
    3. 上海中医药大学中药学院, 上海, 200032
  • Online:2004-11-20 Published:2004-11-20

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摘要： 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。

Abstract: Objective To establish a high-performance liquid chromatography (HPLC) for determining stachydrine and leonurine contents in the crude drug of Yimu Cao, a Chinese motherwort herb(Herba Leonuri, the aerial part of Leonurus japonicus).Methods The sample was obtained from the crude drug by ultrasonic extraction with ethanol after decolorization with ethyl acetate. YMC-Park CN column (250.0 mm×4.6 mm) was used with the mobile phase for stachydrine of 0.001 25 mol/L SDS (containing 0.05% HClO4):C2H5CN (90:10) at the flow rate of 1.5 ml/min with the wavelength for detection of 201.7 nm, and that for leonurine of 0.00125 mol/L SDS (containing 0.05% HClO4):CH3OH (90:10) at the flow rate of 1 ml/min with the wavelength for detection of 282 nm. The sensitivity was 0.1 AUFs and the column temperature was 20℃.Results With the injection amount (mg) as the abscissa and the peak area as the ordinate, the regression equation of the calibration curve for stachydrine was Y=1 187.542 3X-168.982 2, and that for leonurine was Y=5 202.654X-221.141 (r=0.9998) with the linearity scope of 2.5-12.5 mg, detective limit of 0.15 mg, and recovery of (99.03±2.744)%. The analysis of extracted drug samples from 18 regions indicated that the alkaloids contents in Yimu Cao varied significantly, i.e. stachydrine within a range of 0.1%-0.2% while leonurine content, which was much lower, within 0.01%-0.05%. In general, the alkaloid contents were higher in the drug produced in northern China than in those produced in southern China. L. japonicus and the variant L. japonicus albiflorus had total alkaloid contents around 0.3%, which was higher than the contents of other species.Conclusion As a convenient and feasible means for determining the alkaloid contents in Yimu Cao, HPLC produces accurate and reliable results and can be more effective than the formerly used methods.

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