山西产酸枣仁HPLC-UV-ELSD特征图谱及7个化学成分的含量测定  

Study on characteristic chromatogram and contents of seven components in Ziziphi Spinosae Semen in Shanxi by HPLC-UV-ELSD

作　　者：杨馥源 魏洁 王玉龙 杜晨晖 闫艳[1] 秦雪梅[1] YANG Fuyuan;WEI Jie;WANG Yulong;DU Chenhui;YAN Yan;QIN Xuemei(Modern Research Center of Traditional Chinese Medicine,Shanxi University,Taiyuan 030006,China;Shanxi Zhendong Chinese Herbal Development Company;College of Traditional Chinese Medicine and Food Engineering,Shanxi University of Traditional Chinese Medicine)

机构地区：[1]山西大学中医药现代研究中心,太原030006 [2]山西振东道地药材股份有限公司 [3]山西中医药大学中药与食品工程学院

出　　处：《山西医科大学学报》2021年第2期194-200,共7页Journal of Shanxi Medical University

基　　金：国家自然科学基金青年基金项目(81603289,81603251);山西省研究生联合培养基地人才培养项目(2017JD01);山西省科技攻关计划振东专项项目(2016ZD0105);山西省青年科技人员培优计划项目(05);山西省卫生健康委“十大晋药”中药材质量标准规范制定和综合利用研究项目(Zyczl2020007)。

摘　　要：目的采用高效液相色谱法建立酸枣仁的特征图谱,并同时测定酸枣仁7个化学成分的含量。方法收集山西临汾大宁、运城闻喜和晋中榆次3个产地的酸枣仁样品,以乌药碱、木兰花碱、维采宁Ⅱ、斯皮诺素、6-阿魏酰斯皮诺素、酸枣仁皂苷A、酸枣仁皂苷B为指标成分,采用Apollo C18柱(250 mm×4.6 mm,5μm)色谱柱,以乙腈和0.1%甲酸水为流动相进行梯度洗脱,柱温为30℃,流速为1.0 ml/min,紫外检测波长分别为227 nm和335 nm,蒸发光散射检测器(ELSD)漂移管温度105℃。空气体积流量为2.5 L/min。结果建立了酸枣仁的特征图谱,标定了7个共有峰,不同检测波长下特征图谱的相似度为0.979-1,相对保留时间和相对峰面积RSD均小于0.3%。在227 nm波长,以木兰花碱为参照峰,乌药碱的相对保留时间为0.84;在335 nm,以斯皮诺素为参照峰,维采宁Ⅱ,6-阿魏酰斯皮诺素的相对保留时间为0.63和1.35;在蒸发光散射检测器(ELSD)检测条件下,以酸枣仁皂苷A为参照峰,酸枣仁皂苷B的相对保留时间为1.1。不同产地酸枣仁中7个成分含量有明显差异,其中乌药碱、木兰花碱、斯皮诺素、酸枣仁皂苷A 4个成分在榆次产地显著高于大宁和闻喜产地。结论本研究所建立的酸枣仁特征图谱方法操作简单,重复性好,并能同时测定酸枣仁中7个成分含量,可为酸枣仁的质量标准研究提供更加全面的依据。Objective To develop a method for characteristic chromatogram and simultaneous quantification of seven components in Ziziphi Spinosae Semen(ZSS)by high performance liquid chromatography(HPLC).Methods HPLC-UV-ELSD characteristic chromatogram of ZSS was established.In addition,an HPLC method was developed and validated for simultaneous quantification of seven components,including coclaurine,magnoflorine,vicenin Ⅱ,spinosin,6-feruylspinosin,jujuboside A and jujuboside B.Chromatographic separation was achieved with an Apollo C18 column(250 mm×4.6 mm,5μm)at the flow rate of 1 ml/min.Gradient elution was performed with a mobile phase consisting of formic acid in water and acetonitrile.The UV detector wavelength was set at 227 nm and 335 nm.The evaporative light-scattering detector(ELSD)drift tube temperature was 105℃,and the air volume flow rate was 2.5 L/min.Results The seven peaks in ZSS,including coclaurine,magnoflorine,vicenin Ⅱ,spinosin,6-feruylspinosin,jujuboside A and jujuboside B,were marked in characteristic chromatogram.The similarity of the characteristic chromatogram at different detection wavelengths was in the range of 0.979-1,and the RSDs of the relative retention time(RRT)and the relative peak area were less than 0.3%.RRT of coclaurine was 0.84 with magnoflorine as a reference at 227 nm.With spinosyn as a reference at 335 nm,the RRTs of vicenin Ⅱ and 6-feruylspinosin were 0.63 and 1.35,respectively.In addition,the RRT of jujuboside B was 1.1 using ELSD method with jujuboside A as a reference.The contents of 7 components in ZSS were significantly different in different producing areas.The contents of coclaurine,magnoflorine,spinosin and jujuboside A were significantly higher in Yuci than those in Daning and Wenxi.Conclusion A stable and reliable quality evaluation method of ZSS is successfully established,which might provide a reference for quality control of ZSS.

关 键 词：酸枣仁 高效液相色谱-紫外-蒸发光检测 含量测定 特征图谱 

分 类 号：R284[医药卫生—中药学]