CN113624706A - 一种基于光谱联用技术鉴别特级初榨橄榄油的方法 - Google Patents
一种基于光谱联用技术鉴别特级初榨橄榄油的方法 Download PDFInfo
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Abstract
本发明公开了一种基于光谱联用技术鉴别特级初榨橄榄油的方法，采用荧光分光光度计和紫外分光光度计联用，将待测样品在光谱条件：荧光光谱条件为激发波长240‑700 nm，发射波长290‑900 nm，狭缝宽度1‑5 nm，步径长度2‑10nm；紫外光谱条件为波长范围250‑1000 nm，扫描速度120‑600 nm/min下同时检测其三维荧光光谱与紫外光谱，有纯特级初榨橄榄油特征三维荧光光谱，且紫外特征吸光度与纯特级初榨橄榄的相等，则为纯特级初榨橄榄油；否则为掺有其他油品的特级初榨橄榄油，并可对掺入特级初榨橄榄油中其他油品的比例进行精准定量。本发明鉴别方法简单，鉴别速度快，鉴别准确率高，特异性强且能实现精准定量。
Description
技术领域
本发明涉及一种特级初榨橄榄油的鉴别方法，尤其涉及一种基于光谱联用技术鉴别特级初榨橄榄油的方法，并可实现特级初榨橄榄油其他油品的定量检测，属于光谱技术鉴别技术领域。
背景技术
基于橄榄油的加工工艺，理化性质以及成分含量上存在的差异，橄榄油被分成不同品级。特级初榨橄榄油是橄榄油评级中的最高等级。作为地中海饮食的重要组成部分，以其营养、健康和愉悦的感官特性享誉世界。由于其优越的营养成分，如单不饱和脂肪酸、维生素和抗氧成分，特级初榨橄榄油在全世界范围内享有极高的声誉。同时，特级初榨橄榄油也被视为功能食品，因为它可以降低血压，减少动脉堵塞和硬化，修复受损的细胞和组织，对抗癌细胞，降低低密度脂蛋白水平，提高高密度脂蛋白水平，加强细胞膜完整性，缓解哮喘症状。其次还含有大量的活性营养成分，如橄榄苦苷，羟基酪醇，角鲨烯等都具有抗菌、抗氧化、消炎的积极作用。
特级初榨橄榄油卓越的品质具有极高的商业价值。因而被当作造假的目标，在特级初榨橄榄油中掺入橄榄果渣油或其他廉价植物油以获取高额经济利益。近年，国人对特级初榨橄榄油越发的认可，也加剧了特级初榨橄榄油掺假现象的频发。因此发展快速、灵敏、准确的鉴伪技术十分迫切和需要。
目前主要应用的鉴伪技术主要有气相色谱以及各种文献报道的液相色谱、液相质谱联用、近红外光谱、拉曼光谱等方法。官方鉴别方法仍以气质联用技术检测其脂肪酸谱为目标，但该方法样品前处理复杂，尤其是甲酯化过程繁琐且无法实时检测，相应的检测成本也较高；现阶段近红外光谱法虽然省去了磨粉、压片等样品处理与制备过程。相比之下本发明所述的荧光紫外联用光谱法不仅检测速度快且成本低廉，操作简便，可以作为检测食用油掺假的方法。
发明内容
本发明的目的是提供一种基于光谱联用技术鉴别特级初榨橄榄油的方法，不需要任何前处理手段就可以实现对特级初榨橄榄油的快速鉴别以及对特级初榨橄榄油中掺入其他廉价油比例的精确检测，为特级初榨橄榄油的发展以及高品质食用油产业提供可靠保障。
本发明利用荧光和紫外光谱中存在的指纹区和特殊激发发射以及吸收峰的位置，实现对特级初榨橄榄油中掺入橄榄果榨油和其他廉价油的鉴别区分与定量检测，具体方法如下：
（1）确定光谱条件：荧光光谱条件为激发波长240-700 nm，发射波长290-900 nm，狭缝宽度1-5nm，步径2-10nm；紫外光谱条件为波长范围250-1000 nm，扫描速度120-600nm/min。
（2）测定纯特级初榨橄榄油的光谱：采用荧光分光光度计和紫外分光光度计联用，将纯特级初榨橄榄油加入混合溶剂中，然后在步骤（1）光谱条件下测定纯特级初榨橄榄油的三维荧光光谱与紫外光谱，纯特级初榨橄榄的紫外特征峰吸光度为0.6-0.8。混合溶剂为四氢呋喃、乙腈、乙醇、乙酸乙酯、二氧六环的混合溶剂；纯特级初榨橄榄油与混合溶剂的体积比为1:2-1:50。
（3）绘制工作曲线：取掺入质量百分数为5%、10%、20%、40%、60%、80%的橄榄果榨油的特级初榨橄榄油，经紫外光谱检测得到的吸光度为纵坐标，橄榄果榨油的掺入质量百分数为横坐标，得到掺有橄榄果榨油的特级初榨橄榄油的线性方程为y=-0.2676x + 0.2854，R² = 0.9979；x为其他油品的掺入质量百分数，y为吸光度（%）；玉米油、菜籽油、大豆油、花生油的线性方程用同样的方法得到，与橄榄果榨油的相同。
（4）测定样品油的光谱：采用荧光分光光度计和紫外分光光度计联用，将待测样品油加入混合溶剂中，然后在步骤（1）光谱条件下同时检测其三维荧光光谱与紫外光谱，或者直接在步骤（1）光谱条件下同时检测其三维荧光光谱与紫外光谱，有纯特级初榨橄榄油特征三维荧光光谱，且紫外特征峰吸光度为0.6-0.8，与纯特级初榨橄榄的紫外特征峰吸光度相等，则为纯特级初榨橄榄油；否则为掺有其他油品的特级初榨橄榄油。荧光光谱：混合溶剂为四氢呋喃、乙腈、乙醇、乙酸乙酯的混合溶剂；待测样品油与混合溶剂的体积比为1:2-1:50。
（5）掺有其他油品的特级初榨橄榄油中其他油品的定量检测：其他油品掺入质量百分数在1-100%的范围内，将经紫外光谱检测得到掺有其他油品的特级初榨橄榄油的吸光度，结合步骤（3）得到的工作曲线，计算得到掺有其他油品的特级初榨橄榄油中其他油品的含量。其他油品包括橄榄果榨油、玉米油、菜籽油、大豆油、花生油。
本发明采用荧光分光光度计和紫外分光光度计联用技术，可以一步实现对掺假油的定性与定量，相比于单一的光谱技术，本发明可同时得到多种信息，且信息之间可相互验证提升检测精度，不仅检测速度快且成本低廉，操作简便，鉴别准确率高，特异性强，为特级初榨橄榄油安全以及高端食用油产业鉴伪提供可靠技术保障。
具体实施方式
实施例1
（1）取待测油样品0.1ml，加入四氢呋喃、乙腈、乙醇、乙酸乙酯混合溶剂4ml；
（2）荧光分光光度计和紫外分光光度计联用，在荧光分光光度计和紫外分光光度计联用，在光谱检测参数：紫外光谱：波长范围为250-1000 nm，扫描速度300 nm/min；荧光光谱：激发波长250-700nm，发射波长300-800nm，狭缝宽度为2 nm，步径10nm条件下同时检测三维荧光光谱与紫外光谱；
（3）检测结果及判定：与纯特级初榨橄榄油光谱参数比较，整体三维荧光光谱形貌、吸光度为0.78，与纯特级初榨橄榄油无明显差异。判定为特级初榨橄榄油。
实施例2
（1）取特级初榨橄榄油中掺入40%橄榄果榨油得到待测油样品0.2ml，加入四氢呋喃、乙腈、乙醇、乙酸乙酯混合溶剂4ml；
（2）荧光分光光度计和紫外分光光度计联用，在光谱检测参数：紫外光谱：波长范围为250-1000 nm，扫描速度为120-600 nm/min；荧光光谱：激发波长500-700nm，发射波长600-800nm，狭缝宽度为1nm，步径5nm条件下同时检测三维荧光光谱与紫外光谱；
（3）检测结果及判定：与纯特级初榨橄榄油光谱参数比较，整体三维荧光光谱形貌、吸光度为0.36，与纯特级初榨橄榄油存在明显差异。判定为掺假油，依据线性曲线y=-0.2676x + 0.2854准确计算掺入比例为39.5%，与实际掺入比例吻合。
实施例3
（1）取特级初榨橄榄油中掺入35%玉米油的待测油样品4ml；
（2）荧光分光光度计和紫外分光光度计联用，在光谱检测参数：紫外光谱：紫外光谱：波长范围为250-1000 nm，扫描速度为120-600 nm/min；荧光光谱：激发波长450-700nm，发射波长500-800 nm，狭缝宽度为5nm，步径5nm条件下同时检测三维荧光光谱与紫外光谱；
（3）检测结果及判定：与纯特级初榨橄榄油光谱参数比较，整体三维荧光光谱形貌、吸光度为0.37，与纯特级初榨橄榄油存在明显差异。判定为掺假油，依据线性曲线y=-0.2676x + 0.2854准确计算掺入比例为35.2%，与实际掺入比例吻合。
实施例4
（1）取特级初榨橄榄油中掺入36%菜籽油的待测油样品0.5ml，加入四氢呋喃、乙腈、乙醇、乙酸乙酯混合溶剂4ml；
（2）荧光分光光度计和紫外分光光度计联用，在光谱检测参数：紫外光谱：波长范围为250-1000 nm，扫描速度为120-600 nm/min；荧光光谱：激发波长250-600nm，发射波长300-700nm，狭缝宽度为2 nm，步径5nm条件下同时检测三维荧光光谱与紫外光谱；
（3）检测结果及判定：与纯特级初榨橄榄油光谱参数比较，整体三维荧光光谱形貌、吸光度为0.38，与纯特级初榨橄榄油存在明显差异。判定为掺假油，依据线性曲线y=-0.2676x + 0.2854准确计算掺入比例为35.8%，与实际掺入比例吻合。
实施例5
（1）取特级初榨橄榄油中掺入24%大豆油的待测油样品5ml；
（2）荧光分光光度计和紫外分光光度计联用，在光谱检测参数：紫外光谱：紫外光谱：波长范围为250-1000 nm，扫描速度为120-600 nm/min；荧光光谱：激发波长350-700nm，发射波长400-800nmnm，狭缝宽度为5 nm，步径10nm条件下同时检测三维荧光光谱与紫外光谱；
（3）检测结果及判定：与纯特级初榨橄榄油光谱参数比较，整体三维荧光光谱形貌、吸光度为0.35，与纯特级初榨橄榄油存在明显差异。判定为掺假油，依据线性曲线y=-0.2676x + 0.2854准确计算掺入比例为23.7%，与实际掺入比例吻合。
实施例6
（1）取特级初榨橄榄油中掺入48%花生油的待测油样品0.15ml，加入四氢呋喃、乙腈、乙醇、乙酸乙酯混合溶剂5ml；
（2）荧光分光光度计和紫外分光光度计联用，在光谱检测参数：紫外光谱：紫外光谱：波长范围为250-1000 nm，扫描速度为120-600 nm/min；荧光光谱：激发波长550-700nm，发射波长600-800nm，狭缝宽度为2nm，步径10nm条件下同时检测三维荧光光谱与紫外光谱；
（3）检测结果及判定：与纯特级初榨橄榄油光谱参数比较，整体三维荧光光谱形貌、吸光度为0.41，与纯特级初榨橄榄油存在明显差异。判定为掺假油，依据线性曲线y=-0.2676x + 0.2854准确计算掺入比例为47.9%，与实际掺入比例吻合。
Claims (4)
1.一种基于光谱联用技术鉴别特级初榨橄榄油的方法，其特征在于：采用荧光分光光度计和紫外分光光度计联用，将待测样品油加入混合溶剂中，然后在如下光谱条件下同时检测其三维荧光光谱与紫外光谱，或者直接在如下光谱条件下同时检测其三维荧光光谱与紫外光谱，有纯特级初榨橄榄油特征三维荧光光谱，且紫外特征峰吸光度为0.6-0.8，则为纯特级初榨橄榄油；否则为掺有其他油品的特级初榨橄榄油；
光谱条件：荧光光谱条件为激发波长240-700 nm，发射波长290-900 nm，狭缝宽度1-5nm，步径2-10nm；紫外光谱条件为波长范围250-1000 nm，扫描速度120-600 nm/min。
2.根据权利要求1所述一种基于光谱联用技术鉴别特级初榨橄榄油的方法，其特征在于：所述混合溶剂为四氢呋喃、乙腈、乙醇、乙酸乙酯的混合溶剂。
3.根据权利要求1所述一种基于光谱联用技术鉴别特级初榨橄榄油的方法，其特征在于：所述待测样品油与混合溶剂的体积比为1:2-1:50。
4.根据权利要求1所述一种基于光谱联用技术鉴别特级初榨橄榄油的方法，其特征在于：掺有其他油品的特级初榨橄榄油中其他油品的定量检测方法：其他油品掺入质量百分数在1-100%的范围内，掺有其他油品的特级初榨橄榄油的吸光度与其他油品的掺入质量百分数呈如下线性关系：
y=-0.2676x + 0.2854，R² = 0.9979
x为其他油品的掺入质量百分数；y为吸光度（%）；
所述其他油品包括橄榄果榨油、玉米油、菜籽油、大豆油、花生油。
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