凝胶渗透色谱-液质联用法同时测定橄榄油中甾醇和三萜烯二醇
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- 英文论文题名：Simultaneous determination of sterols,erythrodiol and uvaol in olive oils by gel permeation chromatography and liquid chromatography-mass spectrometry
- 论文作者：顾强 ; 乙小娟 ; 刘一军 ; 邵景东
- 英文论文作者：Qiang Gu ; Xiaojuan Yi ; Jin Shi ; Yijun Liu ; Jingdong Shao ; Technology Center ; Zhangjiagang Entry-Exit Inspection and Quarantine Bureau
- 年：2016
- 作者机构：张家港出入境检验检疫局综合技术中心;
- 论文关键词：甾醇 ; 三萜烯二醇 ; 橄榄油 ; 检测 ; 凝胶渗透色谱
- 会议召开时间：2016-07-01
- 会议录名称：中国化学会第30届学术年会摘要集-第二十三分会：复杂样品分离分析
- 语种：中文
- 分类号：O657.63;TS227
- 学会代码：ZGHY
- 会议名称：中国化学会第30届学术年会-第二十三分会 ; 复杂样品分离分析
- 会议地点：中国辽宁大连
- 主办单位：中国化学会
- 学会名称：中国化学会
- 页数：1
- 文件大小：188k
- 原文格式：D
- 会议级别：全国
摘要
橄榄油中甾醇和三萜烯二醇的检测一般需要经皂化、萃取、薄层层析、硅烷化等复杂的前处理步骤后再进行气相色谱测定,不仅操作十分繁琐,而且极为费时。本工作首次将凝胶渗透色谱(GPC)引入到橄榄油中甾醇类物质的检测中,利用GPC将甾醇和三萜烯二醇从橄榄油基质中分离出来,然后采用全自动定量浓缩仪将流出液氮吹干,最后采用液质联用(LC-MS)测定包括高根二醇、熊果醇、麦角固醇、菜籽甾醇、菜油甾醇、岩藻甾醇、豆甾醇、胆固醇、β-谷甾醇等9种物质的含量。我们从线性范围、检出限、定量限、加标回收率、重复性和重现性等多个指标上对本方法进行了验证,证明了方法的可靠性。本方法的特点在于自动化程度高,目标物分离、GPC流出液中溶剂的去除等核心步骤均可由仪器自动完成。仅样品称量、GPC流出液的转移、提取物的复溶等几个简单步骤需要人工操作,每个样品的人工操作时间仅在15 min以内,极大简化了实验步骤,节约了检测时间。
It is well known that the analysis of sterols,erythrodiol and uvaol in olive oils is laborious and time-consuming.In this work,we presented a highly automated method for simultaneous analysis of these compounds with gel permeation chromatography(GPC),automatic solvent evaporator and LC-MS.The olive oils dissolved in mixed solvents were directly injected into GPC.After separating from the olive oils,the target analytes were concentrated by an automatic solvent evaporator.Erythrodiol,uvaol,ergosterol,brassicasterol,cholesterol,fucosterol,campesterol,stigmasterol and β-sitosterol were then quantified by liquid chromatography-mass spectrometry(LC-MS) with an interface of atmospheric pressure chemical ionization(APCI).The method was validated by evaluating the linearity of calibration curves,limits of detection,limits of quantification and precision(including recovery,repeatability and reproducibility).Several real samples were also analyzed by the proposed method,and we found that it only takes 15 minutes of manual operation for each sample.
It is well known that the analysis of sterols,erythrodiol and uvaol in olive oils is laborious and time-consuming.In this work,we presented a highly automated method for simultaneous analysis of these compounds with gel permeation chromatography(GPC),automatic solvent evaporator and LC-MS.The olive oils dissolved in mixed solvents were directly injected into GPC.After separating from the olive oils,the target analytes were concentrated by an automatic solvent evaporator.Erythrodiol,uvaol,ergosterol,brassicasterol,cholesterol,fucosterol,campesterol,stigmasterol and β-sitosterol were then quantified by liquid chromatography-mass spectrometry(LC-MS) with an interface of atmospheric pressure chemical ionization(APCI).The method was validated by evaluating the linearity of calibration curves,limits of detection,limits of quantification and precision(including recovery,repeatability and reproducibility).Several real samples were also analyzed by the proposed method,and we found that it only takes 15 minutes of manual operation for each sample.
引文
[1]Zarrouk,W.;Carrasco-Pancorbo,A.;Zarrouk,M.;et al.Talanta 2009,80:924.
[2]Gu,Q.;Yi,X.;Zhang,Z.;et al.Anal.Methods 2016,DOI:10.1039/C5AY02193F.
[2]Gu,Q.;Yi,X.;Zhang,Z.;et al.Anal.Methods 2016,DOI:10.1039/C5AY02193F.