水飞蓟果实、果皮及其提取物质量评价法的研究

目的建立水飞蓟果实、果皮及其提取物综合质量评价方法。方法用UV法在 2 87nm下测定水飞蓟素的含量 ;并以HPLC法测定指标成分水飞蓟宾的含量 :采用HypersilC1 8(2 5 0mm×4 6mm ,5 μm)色谱柱 ;以甲醇 乙腈 磷酸二氢铵缓冲液 (2 4∶2 4∶5 0 ,pH =5 )为流动相 ;流速为1 0mL min ;柱温为 4 0℃ ;检测波长为 2 87nm。结果UV法和HPLC法线性分别在 8 0 4～4 0 2 μmol L和 0 2 76～ 1 3 8μg;加样回收率 :UV法 98 5 % ,HPLC法 97 3 % ;水飞蓟果实、果皮中水飞蓟素和水飞蓟宾含量分别为 3 88%和 1 3 2 %、8 0 1 %和 2 77% ;3种水飞蓟提取物中水飞蓟素含量均在 80 %以上 ,但水飞蓟宾含量在 2 8 7%～ 3 2 8% ,有明显差异。结论 2法合用可用于水飞蓟原料药材及提取物的质量综合评价和控制

Studies on the quality evaluation of the extracts of truits,skin and their Silybum marianum (L.) Gaertn

Objective To establish the general evaluation of the quality of Silybum marianum (L.)Gaertn.and its extracts from its fruits,skin and extracts.Methods The contents of silymarin were detected at 287 nm by the UV method.In the analysis of silybin by the HPLC method,using the ODS reversed-phase column of Hypersil C 18(4.6 mm× 250 mm, 5 μm),the mobile phase was a combination of methanol,acetonitrile and ammonium dihydrophosphate in the volume ration of 24∶24∶50 at the pH value of 5 at the flowrate of 1.0 mL/min,and the eluate was monitored with UV absorption at 287 nm.Results The linear ranges of silymarin are 8.04～ 40.2 μmol/L with the r= 1.000 and the recovery is 98.5% in the UV determination,while those of the silybin are 0.276～ 1.38 μg with the r= 0.999 7 and the recovery is 97.3% in the HPLC determination.The contents of silymarin and silybin in the fruits or peel of Silybum marianum (L.)Gaertn.collected in Suihua,Heilongjiang Province,are 3.88% and 1.32% or 8.01% and 2.77%,respectively.Although the contents of silymarin in the three commercial samples of its extracts are all more than 80%,but there are clear differences in the silybin contents.Conclusions The combination of both methods may be helpful to the quality control of Silybum marianum (L.)Gaertn. and its extracts.