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基于光谱法的特级初榨橄榄油快速鉴伪技术

唐聪 邵士俊 温玉洁 梁卿 董树清

唐聪,邵士俊,温玉洁,等. 基于光谱法的特级初榨橄榄油快速鉴伪技术[J]. 食品工业科技,2023,44(9):309−316. doi: 10.13386/j.issn1002-0306.2022060131
引用本文: 唐聪,邵士俊,温玉洁,等. 基于光谱法的特级初榨橄榄油快速鉴伪技术[J]. 食品工业科技,2023,44(9):309−316. doi: 10.13386/j.issn1002-0306.2022060131
TANG Cong, SHAO Shijun, WEN Yujie, et al. Rapid Identification of Extra Virgin Olive Oil by Spectrometry[J]. Science and Technology of Food Industry, 2023, 44(9): 309−316. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022060131
Citation: TANG Cong, SHAO Shijun, WEN Yujie, et al. Rapid Identification of Extra Virgin Olive Oil by Spectrometry[J]. Science and Technology of Food Industry, 2023, 44(9): 309−316. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022060131

基于光谱法的特级初榨橄榄油快速鉴伪技术

doi: 10.13386/j.issn1002-0306.2022060131
基金项目: 国家重点研发计划(No.2019YFD1002403);甘肃省重点研发计划(No.20YF8FA003)。
详细信息
    作者简介:

    唐聪(1996−),男,博士研究生,研究方向:油脂鉴别,E-mail:Tangcong@licp.cas.cn

    通讯作者:

    邵士俊(1968−),男,博士,研究员,研究方向:分子识别与分离分析方法研究,E-mail:sjshao@licp.cas.cn

    董树清(1978−),女,博士,副研究员,研究方向:生物分析 、分离分析,E-mail:sqdong@licp.cas.cn

  • 中图分类号: TS227

Rapid Identification of Extra Virgin Olive Oil by Spectrometry

  • 摘要: 本文研究了特级初榨橄榄油中掺入不同比例橄榄果榨油(精炼橄榄油)、菜籽油、玉米油和大豆油的光谱特征,采用荧光光谱和紫外光谱,对掺假样品及纯油样品进行了快速检测。结果表明,特级初榨橄榄油的光谱特征与其他植物油之间差异较大,且掺假体积与吸光度之间存在良好的线性关系(R2>0.89),实现了特级初榨橄榄油的定性鉴别与定量检测,建立了特级初榨橄榄油质量控制体系及其掺假检测分析技术,最低检出限为1%,线性范围为5%~100%(v/v)。系统聚类分析将所有特级初榨橄榄油准确地分为一个亚类,也佐证了此方法的稳定性与可靠性。这种简单快捷的检测技术,有助于特级初榨橄榄油实时、在线橄榄油检测分析技术的研发,为我国橄榄油品质鉴定及产业发展提供有利的技术保障。

     

  • 图  各类植物油的三维荧光光谱图

    注:a,a*:特级初榨橄榄油;b,b*:橄榄果渣油;c,c*:菜籽油;d,d*:玉米油;e,e*:大豆油。

    Figure  1.  3D fluorescence spectrogram of various vegetable oils

    图  掺入不同体积百分比菜籽油的特级初榨橄榄油的三维荧光光谱图

    注:a,a* :0%;b,b* :20%;c,c* :40%;d,d* :80%;e,e* :100%。

    Figure  2.  3D fluorescence spectra of extra virgin olive oil incorporated with different volume percentages of rapeseed oil

    图  各类植物油的发射荧光光谱(a)和可见吸收光谱(b)

    Figure  3.  Emission fluorescence spectrum (a) and UV absorption spectrum (b) of various vegetable oils

    图  掺入不同种类植物油的体积百分数与特级初榨橄榄油(EVOO-1)吸光度的关系

    注:a:RVO-1;b:RVO-3;c:RO;d:CO;e:SO。

    Figure  4.  Relationship between incorporation amount and absorbance of EVOO-1 ked with different oils

    图  掺入油品不同的特级初榨橄榄油的吸光度与掺入体积百分比的标准曲线

    注:a:EVOO-1;b:EVOO-5;c:EVOO-6;d:EVOO-7。

    Figure  5.  Standard curve of absorbance versus volume percent of blended extra virgin olive oil with different blends

    图  各类植物油的系统聚类分析

    Figure  6.  Systematic cluster analysis of various vegetable oils

    表  1  样品信息

    Table  1.   Sample information

    类别序号产地品牌品种加工工艺质量等级
    特级初榨橄榄油EVOO-1甘肃田园鄂植8号冷榨特级初榨
    EVOO-2甘肃田园Leccino冷榨特级初榨
    EVOO-3甘肃祥宇冷榨特级初榨
    EVOO-4山东鲁花冷榨特级初榨
    EVOO-5湖北鑫榄园冷榨特级初榨
    EVOO-6意大利欧丽薇兰冷榨特级初榨
    EVOO-7西班牙贝蒂斯Hojiblanca,Picual冷榨特级初榨
    橄榄果渣油RVO-1意大利欧丽薇兰混合型精炼一级
    RVO-2西班牙西奥图混合型精炼一级
    RVO-3江西念食安混合型精炼一级
    菜籽油RO中国金龙鱼精炼精炼一级
    玉米油CO中国长寿花精炼精炼一级
    大豆油SO中国金龙鱼精炼精炼一级
    注:“−”表示该产品中未注明榨油的油橄榄品种。
    下载: 导出CSV

    表  2  线性拟合度(R2)和精密度(RSD)

    Table  2.   Linear fit (R2) and precision (RSD)

    EVOO-1EVOO-5EVOO-6EVOO-7
    R2RSD(%)R2RSD(%)R2RSD(%)R2RSD(%)
    RVO-10.99280.100.92781.100.98380.400.92683.42
    RVO-30.99570.120.91190.350.98640.970.95170.31
    RO0.99500.190.92640.510.94850.100.95840.98
    CO0.98720.340.89420.210.97140.030.97930.63
    SO0.97751.800.89290.530.96330.610.94390.88
    下载: 导出CSV
  • [1] LOPEZ-MIRANDA J, PEREZ-JIMENEZ F, ROS E, et al. Olive oil and health: Summary of the II international conference on olive oil and health consensus report, Jaen and Cordoba (Spain) 2008[J]. Nutr Metab Cardiovasc Dis,2010,20(4):284−294. doi: 10.1016/j.numecd.2009.12.007
    [2] MENDES T O, DA ROCHA R A, PORTO B L S, et al. Quantification of extra-virgin olive oil adulteration with soybean oil: A comparative study of NIR, MIR, and Raman spectroscopy associated with chemometric approaches[J]. Food Analytical Methods,2015,8(9):2339−2346. doi: 10.1007/s12161-015-0121-y
    [3] ALONSO-SALCES R M, GALLO B, COLLADO M I, et al. 1H-NMR fingerprinting and supervised pattern recognition to evaluate the stability of virgin olive oil during storage[J]. Food Control,2021,123:107831. doi: 10.1016/j.foodcont.2020.107831
    [4] CASADEI E, VALLI E, PANNI F, et al. Emerging trends in olive oil fraud and possible countermeasures[J]. Food Control,2021,124:107902. doi: 10.1016/j.foodcont.2021.107902
    [5] MEENU M, CAI Q, XU B. A critical review on analytical techniques to detect adulteration of extra virgin olive oil[J]. Trends in Food Science & Technology,2019,91:391−408.
    [6] PRESTI G, GIULIANO S, GULOTTA E, et al. Legal blends between olive oil and other vegetable oils: Quantification of olive oil and identification of "virgin olive oils"", refined olive oils" and "olive pomace oils"[J]. Talanta Open,2021,3:100039. doi: 10.1016/j.talo.2021.100039
    [7] 李淑静, 赵婷, 葛含光, 等. 气相色谱-离子迁移谱应用于橄榄油的掺假鉴别[J]. 食品研究与开发,2018,39(15):109−116. [LI Shujing, ZHAO Ting, GE Hanguang, et al. Application of gas chromatography-ion mobility spectrometry to identification of olive oil adulteration[J]. Food Research and Development,2018,39(15):109−116.
    [8] KHEZELI T, DANESHFAR A, SAHRAEI R. A green ultrasonic-assisted liquid-liquid microextraction based on deep eutectic solvent for the HPLC-UV determination of ferulic, caffeic and cinnamic acid from olive, almond, sesame and cinnamon oil[J]. Talanta,2016,150:577−585. doi: 10.1016/j.talanta.2015.12.077
    [9] 马玉华, 唐方东, 刘佳煜, 等. 稳定同位素比技术用于橄榄油的掺假鉴定[J]. 质谱学报,2021,42(2):189−196. [MA Yuhua, TANG Fangdong, LIU Jiayu, et al. Adulteration identification of olive oil by stable isotope ratio technique[J]. Chinese Journal of Mass Spectrometry,2021,42(2):189−196.
    [10] WANG H, WAN X. Effect of chlorophyll fluorescence quenching on quantitative analysis of adulteration in extra virgin olive oil[J]. Spectrochimica Acta-Part A: Molecular and Biomolecular Spectroscopy, 2021, 248(5): 119183.
    [11] VIEIRA L S, ASSIS C, DE QUEIROZ M, et al. Building robust models for identification of adulteration in olive oil using FT-NIR, PLS-DA and variable selection[J]. Food Chem,2021,345:128866. doi: 10.1016/j.foodchem.2020.128866
    [12] RUISANCHEZ I, JIMENEZ-CARVELO A M, CALLAO M. ROC curves for the optimization of one-class model parameters. A case study: Authenticating extra virgin olive oil from a Catalan protected designation of origin[J]. Talanta,2021,222(15):121564.
    [13] 于迎涛, 王季锋, 孙玉叶, 等. 采用降温扰动二维相关拉曼光谱鉴别掺假橄榄油[J]. 光谱学与光谱分析,2020,40(12):3727−3731. [YU Yingtao, WANG Jifeng, SUN Yuye, et al. Identification of adulterated olive oil by two-dimensional correlation Raman spectroscopy with cooling disturbance[J]. Spectroscopy and Spectral Analysis,2020,40(12):3727−3731.
    [14] 黄帅, 王强, 应瑞峰, 等. 拉曼光谱技术在橄榄油掺伪及品质鉴定中的应用研究进展[J]. 食品工业科技,2019,40(11):334−341. [HUANG Shuai, WANG Qiang, YING Ruifeng, et al. Research progress on the application of Raman spectroscopy in olive oil adulteration and quality identification[J]. Food Industry Science and Technology,2019,40(11):334−341. doi: 10.13386/j.issn1002-0306.2019.11.055
    [15] MAJCHRZAK T, WOJNOWSKI W, DYMERSKI T, et al. Electronic noses in classification and quality control of edible oils: A review[J]. Food Chemistry,2018,246(25):192−201.
    [16] SPADAFORA N D, MASCREZ S, MCGREGOR L, et al. Exploring multiple-cumulative trapping solid-phase microextraction coupled to gas chromatography-mass spectrometry for quality and authenticity assessment of olive oil[J]. Food Chemistry,2022,383(30):132438.
    [17] ZHOU X, ZHANG Q, CHEN X, et al. In-situ assessment of olive oil adulteration with soybean oil based on thermogravimetric-gas chromatography/mass spectrometry combined with chemometrics[J]. Food Control,2021,130:108251. doi: 10.1016/j.foodcont.2021.108251
    [18] FASCIOTTI M, PEREIRA NETTO A D. Optimization and application of methods of triacylglycerol evaluation for characterization of olive oil adulteration by soybean oil with HPLC-APCI-MS-MS[J]. Talanta,2010,81(3):1116−1125. doi: 10.1016/j.talanta.2010.02.006
    [19] TOMÉ-RODRÍGUEZ S, LEDESMA-ESCOBAR C A, PENCO-VALENZUELA J M, et al. Cultivar influence on the volatile components of olive oil formed in the lipoxygenase pathway[J]. LWT-Food Science and Technology,2021,147:111485. doi: 10.1016/j.lwt.2021.111485
    [20] 堵锡华, 宋明, 田林, 等. 橄榄油挥发性香气成分的神经网络定量结构-保留相关性(QSRR)研究[J]. 中国粮油学报,2020,35(12):148−155. [DU Xihua, SONG Ming, TIAN Lin, et al. Neural network quantitative structure-retention correlation (QSRR) study of volatile aroma components in olive oil[J]. Chinese Journal of Cereals and Oils,2020,35(12):148−155. doi: 10.3969/j.issn.1003-0174.2020.12.024
    [21] 田维芬, 周君, 明庭红, 等. 基于电子鼻和GC-MS的不同品牌橄榄油挥发性风味物质研究[J]. 食品工业科技,2017,38(7):285−292. [TIAN Weifen, ZHOU Jun, MING Tinghong, et al. Study on volatile flavor compounds of different brands of olive oil based on electronic nose and GC-MS[J]. Food Industry Science and Technology,2017,38(7):285−292. doi: 10.13386/j.issn1002-0306.2017.07.047
    [22] 赵玉, 张玉环, 李建科, 等. GC-O结合OAV鉴定陇南初榨橄榄油关键香气成分[J]. 食品科学,2022,43(8):184−189. [ZHAO Yu, ZHANG Yuhuan, LI Jianke, et al. Identification of key aroma components of Longnan virgin olive oil by GC-O combined with OAV[J]. Food Science,2022,43(8):184−189.
    [23] GÓMEZ-COCA R B, PÉREZ-CAMINO M D C, BRERETON P, et al. Fatty acid ethyl esters (FAEE) in virgin olive oil: A shorter and full validated approach as an alternative to the EU official method[J]. Food Chemistry,2022,394(15):133300.
    [24] 李勇杰, 耿树香, 吴涛, 等. 云南不同引种地油橄榄油脂组成分析[J/OL]. 中国油脂, 2022, 1−10 [2022-08-13] DOI: 10.19902/j.cnki.zgyz.1003-7969.210785.

    LI Yongjie, GENG Shuxiang, WU Tao, et al. Analysis of olive oil composition of different introduced soil oils in Yunnan[J/OL]. China Oils and Fats, 2022, 1−10 [2022-08-13] DOI: 10.19902/j.cnki.zgyz.1003-7969.210785.
    [25] 杨雯懿, 陈林, 周学忠. 基于主成分分析和聚类分析的橄榄油中微量元素的统计比较[J]. 食品与发酵工业,2020,46(14):222−227. [YANG Wenyi, CHEN Lin, ZHOU Xuezhong. Statistical comparison of trace elements in olive oil based on principal component analysis and cluster analysis[J]. Food and Fermentation Industry,2020,46(14):222−227.
    [26] 王强, 王锴, 黄梅桂, 等. LLE-UPLC-FLD法测定橄榄油中羟基酪醇和酪醇的含量[J]. 食品工业科技,2018,39(9):233−238. [WANG Qiang, WANG Kai, HUANG Meigui, et al. Determination of hydroxytyrosol and tyrosol in olive oil by LLE-UPLC-FLD method[J]. Food Industry Science and Technology,2018,39(9):233−238. doi: 10.13386/j.issn1002-0306.2018.09.041
    [27] MOSSOBA M M, AZIZIAN H, FARDIN-KIA A R, et al. First application of newly developed FT-NIR spectroscopic methodology to predict authenticity of extra virgin olive oil retail products in the USA[J]. Lipids,2017,52(5):443−455. doi: 10.1007/s11745-017-4250-5
    [28] DE LIMA T K, MUSSO M, BERTOLDO MENEZES D. Using Raman spectroscopy and an exponential equation approach to detect adulteration of olive oil with rapeseed and corn oil[J]. Food Chemistry,2020,333(15):127454.
    [29] ABAMBA OMWANGE K, AL RIZA D F, SAITO Y, et al. Potential of front face fluorescence spectroscopy and fluorescence imaging in discriminating adulterated extra-virgin olive oil with virgin olive oil[J]. Food Control,2021,124:107906. doi: 10.1016/j.foodcont.2021.107906
    [30] TORRECILLA J S, ROJO E, DOMINGUEZ J C, et al. A novel method to quantify the adulteration of extra virgin olive oil with low-grade olive oils by UV-vis[J]. Journal of Agric Food Chem,2010,58(3):1679−1684. doi: 10.1021/jf903308u
    [31] 张欣, 杨瑞钰, 陈迪, 等. 豆甾二烯用于特级初榨橄榄油掺假检测的研究[J]. 食品工业科技,2014,35(18):80−92. [ZHANG Xin, YANG Ruiyu, CHEN Di, et al. Study on adulteration detection of extra virgin olive oil by stigmasteradiene[J]. Food Industry Science and Technology,2014,35(18):80−92.
    [32] 王哲, 李晨曦, 钱蕊, 等. 二维相关近红外光谱的植物油鉴别方法[J]. 光谱学与光谱分析,2020,40(10):3230−3234. [WANG Zhe, LI Chenxi, QIAN Rui, et al. Identification method of vegetable oil by two-dimensional correlation near-infrared spectroscopy[J]. Spectroscopy and Spectral Analysis,2020,40(10):3230−3234.
    [33] CABRERA-BAÑEGIL M, MARTÍN-VERTEDOR D, BOSELLI E, et al. Control of olive cultivar irrigation by front-face fluorescence excitation-emission matrices in combination with PARAFAC[J]. Journal of Food Composition and Analysis,2018,69:189−196. doi: 10.1016/j.jfca.2018.01.021
    [34] 王泓鹏, 万雄, 袁汝俊. 基于超连续光谱特级初榨橄榄油的快速检测方法[J]. 光谱学与光谱分析,2020,40(4):1251−1256. [WANG Hongpeng, WAN Xiong, YUAN Rujun. Rapid detection method of extra virgin olive oil based on supercontinuum spectroscopy[J]. Spectroscopy and Spectral Analysis,2020,40(4):1251−1256.
    [35] 许荣辉, 汪勇先, 贾广强, 等. CdS纳米晶的稳定化处理及介质极性对荧光光谱的影响[J]. 人工晶体学报,2006,35(6):1341−1345. [XU Ronghui, WANG Yongxian, JIA Guangqiang, et al. Stabilization of CdS nanocrystals and influence of medium polarity on fluorescence spectra[J]. Journal of Synthetic Crystals,2006,35(6):1341−1345. doi: 10.3969/j.issn.1000-985X.2006.06.039
    [36] 龙伶俐, 薛雅琳, 张蕊, 等. 利用紫外吸收光谱研究植物油精炼程度[J]. 农业机械,2012,24:61−63. [LONG Lingli, XUE Yalin, ZHANG Rui, et al. Study on the degree of vegetable oil refining by ultraviolet absorption spectroscopy[J]. Agricultural Machinery,2012,24:61−63. doi: 10.16167/j.cnki.1000-9868.2012.24.002
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