高效液相色谱-双波长法测定黄精中5种活性化学成分的含量  

Determination of 5 Active Chemical Constituents in Polygonatum Sibiricum Red.by High Performance Liquid Chromatography with Dual Wavelengths

作　　者：刘彦东[1] 黄俊学[1] 张权[2] 梁茜 陈文生[1] LIU Yandong;HUANG Junxue;ZHANG Quan;LIANG Xi;CHEN Wensheng(Guizhou Provincial Key Laboratory of Information System of Mountainous Areas and Protection of Ecological Environment, Testing and Analysis Center, Guizhou Normal University, Gui yang 550001, China;Guizhou Provincial Center for Disease Control and Prevention, Guiyang 550004, China)

机构地区：[1]贵州师范大学分析测试中心贵州省山地环境信息系统与生态保护重点实验室,贵阳550001 [2]贵州省疾病预防控制中心,贵阳550004

出　　处：《理化检验（化学分册）》2018年第4期398-402,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：贵州省科技厅科学技术基金项目(黔科合J字LKS[2013]08号)

摘　　要：提出了高效液相色谱-双波长法同时测定不同生长期的黄精中腺苷、人参皂苷Rb1、β-谷甾醇、香草酸和甘草素等5种活性化学成分含量的方法。样品5.000 0g经甲醇(70+30)溶液40mL超声提取30min,提取液以Diamonsil钻石C_(18)色谱柱为固定相,以0.1%(体积分数)甲酸溶液和0.1%(体积分数)甲酸-乙腈溶液的混合液为流动相进行梯度洗脱,双波长检测(λ_1=252nm,λ_2=280nm)。在优化的试验条件下,5种活性化学成分的质量浓度在0.5~100mg·L^(-1)范围内与其峰面积呈线性关系,检出限(3S/N)为0.36~0.47mg·kg^(-1)。按标准加入法进行回收试验,回收率在96.0%~101%之间,其相对标准偏差(n=6)均小于3.0%。A method of simultaneous determination of 5 active chemical constituents（adenosine,ginsenoside Rb1,β-sitosterol,vanillic acid and liquiritigenin）in Polygonatum Sibiricum Red.at different growth stages was proposed by high performance liquid chromatography with dual wavelengths.The sample（5.000 0 g）was extracted ultrasonically for 30 min with 40 mL of methanol（70＋30）solution.The extract was separated by HPLC with dual wavelengths（λ1=252 nm,λ2=280 nm）using Diamonsil C18 column as the stationary phase,and a mixture of 0.1%（φ）formic acid solution and 0.1%（φ）formic acid-acetonitrile solution in different volume ratios as the mobile phase for gradient elution.Under the optimized test conditions,linear relationships between values of peak area and mass concentration of 5 active chemical constituents were found in the range of 0.5^-100 mg·L^-1,with detection limits（3 S/N）in the range of 0.36-0.47 mg·kg^-1.Test for recovery was made by standard addition method,giving results in the range of 96.0%^-101% and RSDs（n=6）all less than 3.0%.

关 键 词：高效液相色谱法 双波长 黄精 化学成分 

分 类 号：O652.63[理学—分析化学]