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目的:建立不同产地、不同部位的野生与栽培广东紫珠中抗凝血活性成分2α,3α,19α,23-四羟基熊果~(-1)2-烯-28-O-β-D-吡喃葡萄糖苷和2α,3α,19α-三羟基齐墩果~(-1)2-烯-28-O-β-D-吡喃葡萄糖苷的薄层鉴别和水苏碱含量测定的方法。方法:TLC法,展开剂为三氯甲烷-甲醇-甲酸(5∶1∶0.1),显色剂为10%硫酸乙醇溶液;HPLC-ELSD法,采用Hypersil-NH_2色谱柱(250 mm×4.6 mm,5μm),以乙腈-水(17∶83)为流动相,流速1.0 m L·min~(-1),柱温30℃,漂移管温度75℃,载气流速2.0 L·min~(-1)。结果:广东紫珠药材及对照药材中2个三萜的TLC分离效果均较好;HPLC-ELSD法测得盐酸水苏碱进样量在0.091 2～0.912μg范围内与峰面积呈现良好的线性关系(r=0.999 9),平均回收率为98.3%(RSD=1.3%),精密度、稳定性良好。不同产地广东紫珠水苏碱的含量有一定的差异,且叶含量高于茎枝含量,栽培含量高于野生含量。结论:此方法简便易行,重复性好,可作为广东紫珠药材质量控制指标。
OBJECTIVE: To establish the anti-coagulation active ingredients 2α, 3α, 19α, 23-tetrahydroxyarsugar ~ (-1) 2-ene-28-O-β- Identification of the glucopyranoside and 2α, 3α, 19α-trihydroxyl oleaneto ~ (-1) 2-en-28-O-β-D-glucopyranoside thin layer identification and stachydrine content determination method. Methods: The TLC method was developed with chloroform-methanol-formic acid (5:1:1.1) and the color reagent as 10% sulfuric acid in ethanol. The HPLC-ELSD was performed on a Hypersil-NH 2 column (250 mm × 4.6 mm , 5μm) with acetonitrile-water (17:83) as the mobile phase at a flow rate of 1.0 m L · min -1 at a column temperature of 30 ℃, a drift tube temperature of 75 ℃ and a carrier gas flow rate of 2.0 L · min ~ 1). Results: TLC analysis of two triterpenes in Radix et Rhizoma Rhei and control herbs was better. The HPLC-ELSD method showed that the injection volume of stachydrine hydrochloride showed a good linearity with the peak area in the range of 0.091 2 ~ 0.912 μg (R = 0.999 9), the average recovery was 98.3% (RSD = 1.3%), precision and good stability. There are some differences in the content of Stachydrine in Guangdong purple pearl in different areas, and the contents of leaves are higher than those of stems and branches, and the content of leaves is higher than that of wild ones. Conclusion: This method is simple, reproducible and can be used as quality control index of Radix.