食用油掺伪的~1H NMR判别
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摘要
【目的】建立新的食用油掺伪判别方法,为掺伪食用油的快速鉴定和监管提供支持。【方法】以63份常见的菜籽油、玉米油、大豆油、花生油、棉籽油、葵花籽油、芝麻油、棕榈油等食用油为研究对象,利用已知正品食用油1 H NMR谱中各信号峰的积分面积,选取其中2组或3组积分面积制作标准图,建立不同种类正品食用油图谱库,用同样的方法对未知食用油进行测试,将得到的数据代入相应标准食用油图谱进行对比以鉴别是否掺伪。【结果】利用2组积分面积得到的二维图谱能够对食用油的种类进行分类判别;利用3组积分面积制作三维图,能够对掺伪食用油进行准确判别,可准确判别的最低掺伪量为24mL/L。所建立的判别方法对各种磁场强度的核磁共振波谱仪检测得到的数据均可采用,而且该方法所用软件简单易用、成本较低。【结论】基于1 H NMR的掺伪食用油判别方法简单、快捷、经济,值得推广应用。
【Objective】This study established a simple and accurate method to discriminate the edible oils adulteration.【Method】~1H NMR spectrum of 63 authentic edible oil samples including rapeseed oils,corn oils,soybean oils,peanut oils,cottonseed oils,sunflower oils,sesame oils and palm oils were obtained by the NMR spectrometer and the integral of each signal peak was estimated.Then,two or three integral values of the signal peaks were used to establish 2 Dor 3 Dstandard diagrams as authentic edible oils databases.Afterwards,the integral values of unknown edible oils were obtained and distinguished by comparing with the standard database.【Result】The two integral values of the peaks in ~1H NMR can distinguish the category of edible oils.The three integral values of the peaks in ~1H NMR can discriminate the adulteration of edible oils with the lowest determination limit of 24 mL/L.Compared to the literature,the advantage of this method was the wide application.All data could be used even they were obtained from the instruments with different magnetic field intensities.Furthermore,the software was inexpensive and easy to use.【Conclusion】In conclusion,this study established a simple,quick and economic method to discriminate the adulteration of edible oils.
【Objective】This study established a simple and accurate method to discriminate the edible oils adulteration.【Method】~1H NMR spectrum of 63 authentic edible oil samples including rapeseed oils,corn oils,soybean oils,peanut oils,cottonseed oils,sunflower oils,sesame oils and palm oils were obtained by the NMR spectrometer and the integral of each signal peak was estimated.Then,two or three integral values of the signal peaks were used to establish 2 Dor 3 Dstandard diagrams as authentic edible oils databases.Afterwards,the integral values of unknown edible oils were obtained and distinguished by comparing with the standard database.【Result】The two integral values of the peaks in ~1H NMR can distinguish the category of edible oils.The three integral values of the peaks in ~1H NMR can discriminate the adulteration of edible oils with the lowest determination limit of 24 mL/L.Compared to the literature,the advantage of this method was the wide application.All data could be used even they were obtained from the instruments with different magnetic field intensities.Furthermore,the software was inexpensive and easy to use.【Conclusion】In conclusion,this study established a simple,quick and economic method to discriminate the adulteration of edible oils.
引文
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[21]Longobardi F,Ventrella A,Napoli C,et al.Classification of olive oils according to geographical origin by using 1 H NMR fingerprinting combined with multivariate analysis[J].Food Chemistry,2012,130(1):177-183.
[22]Agiomyrgianaki A,Petrakis P V,Dais P.Detection of refined olive oil adulteration with refined hazelnut oil by employing NMR spectroscopy and multivariate statistical analysis[J].Talanta,2010,80(5):2165-2171.
[23]Alonso-Salces R M,Héberger K,Holland M V,et al.Multivariate analysis of NMR fingerprint of the unsaponifiable fraction of virgin olive oil for authentication purposes[J].Food Chemistry,2010,118(4):956-965.
[24]Fragaki G,Spyros A,Siragakis G,et al.Detection of extra virgin olive oil adulteration with lampante olive oil and refined olive oil using nuclear magnetic resonance spectroscopy and multivariate statistical analysis[J].J Agric Food Chem,2005,53(8):2810-2816.
[25]D’Imperio M,Gobbino M,Picanza A,et al.Influence of harvest methodand period on olive oil composition:an NMR and statistical study[J].J Agric Food Chem,2010,58(20):11043-11051.
[2]Fernandes G,Venkatraman J T.Role of omega-3fatty acids in health and disease[J].Nutr Res,1993,13(S1):19-45.
[3]Barison A,da Silva C W P,Campos F R,et al.A simple methodology for the determination of fatty acid composition in edible oils through 1 H NMR spectroscopy[J].Magn Res Chem,2010,48(8):642-650.
[4]Craske J D,Bannon C D.Gas liquid chromatography analysis of the fatty acid composition of fats and oils:a total system for high accuracy[J].J Am Oil Chem Soc,1987,64(10):1413-1417.
[5]Sacchi R,Medina I,Aubourg S P,et al.Proton nuclear magnetic resonance and structure-specific determination of omega-3polyunsaturated fatty acids in fish lipids[J].J Am Oil Chem Soc,1993,70(3):225-228.
[6]Igarashi T,Aursand M,Hirata Y,et al.Nondestructive quantitative determination of docosahexaenoic acid and n-3fatty acids in fish oils by high-resolution 1 H nuclear magnetic resonance spectroscopy[J].J Am Oil Chem Soc,2000,77(7):737-748.
[7]Liu C L,Pan D D,Ye Y F,et al.1 H NMR and multivariate data analysis of the relationship between the age and quality of duck meat[J].Food Chemistry,2013,141(2):1281-1286.
[8]Consonni R,Cagliani L R,Benevelli F,et al.NMR and chemometric methods:apowerful combination for characterization of balsamic and traditional balsamic vinegar of modena[J].Anal Chim Acta,2008,611(1):31-40.
[9]Duarte I,Barros A,Belton P S,et al.High-resolution nuclear magnetic resonance spectroscopy and multivariate analysis for the characterization of beer[J].J Agric Food Chem,2002,50(9):2475-2481.
[10]Consonni R,Gatti A.1 H NMR studies on Italian balsamic and traditional balsamic vinegars[J].J Agric Food Chem,2004,52(11):3446-3450.
[11]Consonni R,Cagliani L R,Cogliati C.NMR characterization of saccharides in Italian honeys of different floral sources[J].J Agric Food Chem,2012,60(18):4526-4534.
[12]Rodrigues J A,Barros A S,Carvalho B,et al.Probing beer aging chemistry by nuclear magnetic resonance and multivariate analysis[J].Anal Chim Acta,2011,702(2):178-187.
[13]Almeida C,Duarte I F,Barros A,et al.Composition of beer by1 H NMR spectroscopy:effects of brewing site and date of production[J].J Agric Food Chem,2006,54(3):700-706.
[14]Michlander E,Peshlov B,Purslow P P,et al.NMR-cooking:monitoring the changes in meat during cooking by low-field1 H-NMR[J].Trends in Food Science&Technology,2002,13(9/10):341-346.
[15]Vigli G,Philippidis A,Spyros A,et al.Classification of edible oils by employing 31Pand 1 H NMR spectroscopy in combination with multivariate statistical analysis:aproposal for the detection of seed oil adulteration in virgin olive oils[J].J Agric Food Chem,2003,51(19):5715-5722.
[16]Mavromoustakos T,Zervou M,Bonas G,et al.A novel analytical method to detect adulteration of virgin olive oil by other oils[J].J Am Oil Chem Soc,2000,77(4):405-411.
[17]Hidalgo F J,Zamora R.Edible oil analysis by high-resolution nuclear magnetic resonance spectroscopy:recent advances and future perspectives[J].Trends Food Sci Technol,2003,14(12):499-506.
[18]Knothe G,Kenar J A.Determination of the fatty acid profile by 1 H-NMR spectroscopy[J].Eur J Lipid Sci Technol,2004,106(2):88-96.
[19]蔡波太,袁龙飞,周影,等.基于1 H NMR指纹图谱结合多变量分析的地沟油检测方法[J].中国科学:化学,2013,43(5):558-567.Cai B T,Yuan L F,Zhou Y,et al.Identification of illegal cooking oils by using 1 H NMR fingerprints combined with multivariate analysis[J].Scientia Sinica Chimica,2013,43(5):558-567.
[20]Dais P,Hatzakis E.Quality assessment and authentication of virgin olive oil by NMR spectroscopy:a critical review[J].Anal Chim Acta,2013,765:1-27.
[21]Longobardi F,Ventrella A,Napoli C,et al.Classification of olive oils according to geographical origin by using 1 H NMR fingerprinting combined with multivariate analysis[J].Food Chemistry,2012,130(1):177-183.
[22]Agiomyrgianaki A,Petrakis P V,Dais P.Detection of refined olive oil adulteration with refined hazelnut oil by employing NMR spectroscopy and multivariate statistical analysis[J].Talanta,2010,80(5):2165-2171.
[23]Alonso-Salces R M,Héberger K,Holland M V,et al.Multivariate analysis of NMR fingerprint of the unsaponifiable fraction of virgin olive oil for authentication purposes[J].Food Chemistry,2010,118(4):956-965.
[24]Fragaki G,Spyros A,Siragakis G,et al.Detection of extra virgin olive oil adulteration with lampante olive oil and refined olive oil using nuclear magnetic resonance spectroscopy and multivariate statistical analysis[J].J Agric Food Chem,2005,53(8):2810-2816.
[25]D’Imperio M,Gobbino M,Picanza A,et al.Influence of harvest methodand period on olive oil composition:an NMR and statistical study[J].J Agric Food Chem,2010,58(20):11043-11051.