摘要
酸枣仁具有显著的改善睡眠和抗焦虑等作用,其提取物在助眠类功能食品开发中应用前景广阔。但目前市场上酸枣仁提取物质量参差不齐,缺乏统一标准,企业在使用时面临较大的质量风险,因此亟须建立一种准确、全面的内控质量评价方法。针对酸枣仁提取物中黄酮和皂苷两类主要活性成分紫外响应差异巨大且水提物中皂苷成分含量低的问题,该研究建立了酸枣仁水提物HPLC定量指纹图谱方法,共标定了8个共有峰。通过对照品指认、文献比对以及高效液相色谱-四极杆飞行时间质谱数据解析,8个共有峰均为黄酮类化合物,该方法可同时实现7种黄酮成分的半定量对比分析和斯皮诺素的含量测定;采用超高效液相色谱-三重四极杆质谱,在正离子模式下,以多反应监测扫描方式可实现酸枣仁皂苷A和B的含量测定;最终以雷达图展现上述10种成分的半定量和定量数据。应用上述方法,该研究对比分析了实验室自制的3批酸枣仁水提物和15家供应商的15批提取物样品。结果显示,实验室自制的3批酸枣仁水提物虽然原料来自不同饮片企业,但总体差异性不大,而不同厂家提供的酸枣仁提取物样品成分含量差异巨大,提示不同厂家存在辅料稀释、理枣仁掺假和醇提或纯化富集等情况。该法为企业制定内控质量标准和筛选合格供应商提供了依据。
Ziziphi Spinosae Semen is the dried seeds of Ziziphus jujuba Mill.var.spinosa(Bunge)Hu ex H.F.Chou,and its extract has broad application prospects in the development of sleep-aid functional foods.However,the quality parameters of Ziziphi Spinosae Semen extracts currently available in the market are not uniform and there is a lack of unified standards.Therefore,it is important to establish an accurate and comprehensive method for quality evaluation.In view of the problems that the UV responses of flavonoids and saponins in the Ziziphi Spinosae Semen extracts vary dramatically and the saponin content in Ziziphi Spinosae Semen water extract is very low,high performance liquid chromatography(HPLC)was used to establish the fingerprint and quantify spinosin.The separation was carried out on a Waters XSelect HSS C18 column(250 mm×4.6 mm,5μm),and the mobile phase was acetonitrile-0.1%(v/v)phosphoric acid aqueous solution for gradient elution.The eight common peaks in the fingerprint of the Ziziphi Spinosae Semen extracts,identified by HPLC-quadrupole time-of-flight mass spectrometry,were attributed to flavonoids by reference substance identification,literature comparison,and high-resolution mass spectrometry data analysis.Semi-quantitative analysis of seven flavonoids and quantitative analysis of spinosin were conducted using the established HPLC quantitative fingerprint.The contents of jujuboside A and jujuboside B were determined by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry.Chromatographic separation was performed on a Waters ACQUITY UPLC BEH C18 column(50 mm×2.1 mm,1.7μm)by gradient elution using a mobile phase of acetonitrile-0.1%(v/v)formic acid aqueous solution.The target compounds were analyzed in multiple reaction monitoring mode with positive electrospray ionization.The semi-quantitative and quantitative data of the above-mentioned 10 components are displayed in the form of radar.Using the above methods,three batches of Ziziphi Spinosae Semen water extracts prepared in
作者
郭秀洁
李昊虬
冯昊天
戚华文
张露
徐伟
伍言娟
王超然
梁鑫淼
GUO Xiujie;LI Haoqiu;FENG Haotian;QI Huawen;ZHANG Lu;XU Wei;WU Yanjuan;WANG Chaoran;LIANG Xinmiao(Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;DICP-CMC Innovation Institute of Medicine, Taizhou 225300, China;Inner Mongolia Dairy Technology Research Institute Co. Ltd., Huhehaote 010110, China;Inner Mongolia Yili Industrial Group Co. Ltd., Huhehaote 010110, China)
出处
《色谱》
CAS
CSCD
北大核心
2021年第9期989-997,共9页
Chinese Journal of Chromatography
基金
江苏省双创团队项目.
关键词
高效液相色谱
质谱
定量指纹图谱
酸枣仁提取物
雷达图
high performance liquid chromatography(HPLC)
mass spectrometry(MS)
quantitative fingerprint
Ziziphi Spinosae Semen extracts
radar-gram
