高效液相色谱法测定土茯苓药材中7种活性成分的含量

Simultaneous determination of seven bioactive constituents in Smilacis Glabrae Rhizoma by high-performance liquid chromatography

建立同时测定土茯苓中(-)-表儿茶素、5-O-咖啡酰基莽草酸、新落新妇苷、落新妇苷、新异落新妇苷、异落新妇苷和黄杞苷含量的高效液相色谱法。采用Agilent Zorbax SB-C18色谱柱(250 mm×4.6 mm,5μm),柱温35℃,流动相为乙腈(B)-0.05%磷酸(A)梯度洗脱,流速1.0 m L·min-1,检测波长230 nm,对土茯苓、短柱肖菝葜、华肖菝葜药材进行分析。测定的84份土茯苓药材中(-)-表儿茶素、5-O-咖啡酰基莽草酸、新落新妇苷、落新妇苷、新异落新妇苷、异落新妇苷和黄杞苷的含量范围分别为trace^1.381,trace^9.913,trace^3.673,0.670 6~27.08,trace^1.181,trace^4.833,trace^2.754 mg·g-1。用建立的方法对土茯苓常见混淆品短柱肖菝葜、华肖菝葜进行分析,结果显示短柱肖菝葜、华肖菝葜药材中(-)-表儿茶素的含量范围分别为0.011 63~0.060 07 mg·g-1和0.015 83~0.085 85 mg·g-1;而其他6种成分均未检测到。该方法简便、准确,可作为土茯苓药材的质量控制方法。短柱肖菝葜和华肖菝葜的成分显著不同于土茯苓,不宜与土茯苓混用。

This study is to develop an HPLC method for the simultaneous determination of （ - ）-epicatechin, 5-O-caffeoylshikimic acid, neoisoastilbin, astilbin, neoisoastilbin, isoastilbin and engeletin in Smilacis Glabrae Rhizoma. Samples of Smilacis Glabrae Rhi- zoma, Heterosmilacis Chinensis Rhizoma and Heterosmilacis Yunnanensis Rhizoma were separated on an Agilent Zorbax SB-C18 column with gradient elution of acetonitrile-0.05% phosphoric acid at a flow rate of 1.0 mL · min-1. The detected wavelength was set at 230 nm and the column temperature was maintained at 35 ℃. The contents of （ - ）-epicatechin, 5-O-caffeoylshikimic acid, neoastilbin, astilbin, neoisoastilbin, isoastilbin and engeletin in 84 Smilacis Glabrae Rhizoma samples were in the range of trace-1. 381, trace- 9.913, trace-3. 673, 0.670 6-27.08, trace-1. 181, trace-4. 833 and trace-2. 754 mg·g-1 respectively. The established method was used for analysis of common adulterants. The results demonstrated that the contents of （ - ） -epicatechin in Heterosmilacis Yunnanensis Rhizoma and Heterosmilacis Chinensis Rhizoma were 0.011 63-0. 060 07 mg·g-1 and 0. 015 83-0. 085 85 mg·g-1, respectively, while the other six constituents were not detected. The method is simple and accurate, and can be used for the quality control of Smilacis Glabrae Rhizoma. The constituents of Heterosmilacis Yunnanensis Rhizoma and Heterosmilacis Chinensis Rhizoma are significantlydifferent from Smilacis Glabrae Rhizoma, and they are not suitable for using as Smilacis Glabrae Rhizoma.