基质固相分散萃取-高效液相色谱法同时测定五味子中5种木脂素类化合物  

Simultaneous determination of five lignans from Schisandra chinensis by matrix solid-phase dispersion extraction-high performance liquid chromatography

作　　者：杜昕昕 王寅鹏 肖伟[2] 朱靖博[1,2] DU Xinxin;WANG Yinpeng;XIAO Wei;ZHU Jingbo(School of Food Science and Technology,Dalian Polytechnic University,Dalian 116034,China;State Key Laboratory of New-tech for Chinese Medicine Pharmaceutical Process,Lianyungang 222001,China)

机构地区：[1]大连工业大学食品学院,辽宁大连116034 [2]中药制药过程新技术国家重点实验室,江苏连云港222001

出　　处：《色谱》2023年第3期257-264,I0003,共9页Chinese Journal of Chromatography

基　　金：国家自然科学基金-联合基金项目(U1603285)。

摘　　要：研究建立了基质固相分散萃取-高效液相色谱(MSPD-HPLC)分析五味子中5种木脂素类化合物(五味子醇甲、五味子醇乙、五味子甲素、五味子乙素、五味子丙素)的方法。采用反相C_(18)色谱柱进行分离,以0.1%(v/v)甲酸水溶液和乙腈为流动相进行梯度洗脱,在波长250 nm下检测。考察了包括硅胶、酸性氧化铝、中性氧化铝、碱性氧化铝、佛罗里硅土、Diol、XAmide、Xion和C_(18)、C_(18)-ME、C_(18)-G_(1)、C_(18)-HC等在内的12种吸附剂以及吸附剂的质量、洗脱剂的种类、洗脱剂体积对五味子木脂素类化合物得率的影响。选定Xion作为MSPD-HPLC分析五味子中木脂素类化合物的吸附剂;基于吸附剂Xion的萃取参数优化结果表明:以0.25 g五味子粉末为固定值,Xion(0.75 g)为吸附剂,甲醇(15 mL)为洗脱剂,MSPD对五味子中木脂素类化合物具有较高的得率。建立的五味子中5种木脂素类化合物的分析方法,各目标分析物具有良好的线性关系(相关系数R^(2)≥0.9999),检出限与定量限分别介于0.0089~0.0294μg/mL和0.0267~0.0882μg/mL之间。对五味子木脂素类化合物进行低、中、高3个水平的加标回收试验,平均回收率为92.2%~111.2%,相对标准偏差为0.23%~3.54%。日内和日间精密度均小于3.6%。与超声辅助提取和热回流提取前处理相比,MSPD具有萃取和净化相结合、耗时少、所需溶剂量少的优点,且MSPD-HPLC获得的结果优于经典方法。所建立的方法成功应用于17批五味子中5种木脂素类化合物含量的分析。The kidney-shaped,red-colord fruit from the plant,Schisandra chinensis(Turcz.)Baill,which belongs to the Schisandraceae family,is among the most popular remedies used in traditional Chinese medicine.The English name of the plant is“Chinese magnolia vine”.It has been used in Asia since ancient times to treat a variety of ailments,including chronic cough and dyspnea,frequent urination,diarrhea,and diabetes.This is because of the wide range of bioactive constituents,such as lignans,essential oils,triterpenoids,organic acids,polysaccharides,and sterols.In some cases,these constituents affects the pharmacological efficacy of the plant.Lignans with a dibenzocyclooctadiene-type skeleton are considered to be the major constituents and main bioactive ingredients of Schisandra chinensis.However,because of the complex composition of Schisandra chinensis,the extraction yields of lignans are low.Thus,it is particularly important to study pretreatment methods used during sample preparation for the quality control of traditional Chinese medicine.Matrix solid-phase dispersion extraction(MSPD)is a comprehensive process involving destruction,extraction,fractionation,and purification.The MSPD method is simple,it requires only a small number of samples and solvents,it does not require any special experimental equipments or instruments,and it can be used to prepare liquid,viscous,semi-solid,solid samples.In this study,a method combining matrix solid-phase dispersion extraction with high performance liquid chromatography(MSPD-HPLC)was established for the simultaneous determination of five lignans(schisandrol A,schisandrol B,deoxyschizandrin,schizandrin B,and schizandrin C)in Schisandra chinensis.The target compounds were separated on a C_(18)column with a gradient elution of 0.1%(v/v)formic acid aqueous solution and acetonitrile as the mobile phases,and detection was performed at a wavelength of 250 nm.First,the effects of 12 adsorbents,including silica gel,acidic alumina,neutral alumina,alkaline alumina,Florisil,Diol,XAmide,Xion,

关 键 词：基质固相分散萃取 高效液相色谱 木脂素类化合物 五味子 

分 类 号：O658[理学—分析化学]