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Olive Oil-Authentication of European Olive Oils

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Olive Oil-Authentication of European Olive Oils Olive Oil-Authentication of European Olive Oils Dr. Christian Gertz Hagen/Germany Authentication • Adulteration – Replacement of high cost ingredients with lower grad and cheaper substitutes • Mislabelling (geographic origin) • Misleading („Bio-, extra virgin, refining“) 1 Detection of Adulterations of Olive oil with Foreign Oils Chemical Parameters Proposed for Authentication of Olive oil • Chromatographic techniques: • Fatty acids (Aparicio et al, 1987) • Fatty acids and sterols (Spangenberg, et al 1998, Stefanoudaki et al (1999), Forina et al 1983, Diaz et al (2005), Arena (2007), • Fatty acids, fatty alcohols and triterpenes (Bianchi et al (2001) • Sterols, triterpenic alcohols and hydrocarbons (Aparicio 1990) • Triacylglycerols (Damiani et al 1997, Gomez-Ariza 2006) • Fatty acids and Triacylglycerols (Tsimidou et al 1987) • Volatile Compounds (Luna et al(2006) • Other techniques: • NIR spectra (Bertran et al 2000, Galtier 2007) • High field H NMR (Mannina et al 2001,Caprone et al 2000, • PTR-MS Araghipour (2008) • HS-MS Lopez Feria (2008) 2 OLIV-TRACK 2002 „Traceability of origin and authenticity of olive oil by combined genomic and metabolomic approaches (EU research programm QLK1-CT-2002-02386) : To ensure traceability of origin and authenticity of olive oil produced and sold within the European Union Triglycerides 3 2 NTAG= 0.5 ( N FA + N FA) Number of individual theoretical number of fatty acids formed TAGs 10 550 12 936 15 1800 3 GLC Conditions for the determination of individual TAGs Stationary Phase: – Restek Rtx 65TG, 0,25 mm ID, 0,1 µm, Column length: 30 m* Supplier.Restek GmbH, Schabenweg 23, 61348 Bad Homburg, Germany (www.restek.com) Oven: Temperature programming: 170 °C (not 300 °C) up to 350 °C (10°C/min; keep 10 min. at 360 °C; Injection/detector temp.: 360 °C; Split: 10:1; Carrier Gas: Hydrogen. HPLC and CGC Separation of Individual TAGs in Olive Oil Official HPLC Method (CR EC 796) CGC Separation DGF C-VI 14 OLO POL/SLL POP OOO POP OOO 4 Analytical Procedures:TG analysis • Method: DGF C-VI 14(08) • Column: • Restek Rtx-65TG, 0,25mm, 30 m, 0,1 µm • Temp. Not 300-360 °C/2°C/min • better: GLC-separation of the individual TAGs (Standard: Sesamoil) Low starting oven temperature to protect the column: Oven Temperature Programm 150 to 320 °C 5 GLC Analysis of FAME According to DGF Standard Method (C4-C26) – Oven temperature: • 120 °C,0min,4°C/Min auf 240 °C, 7 min – Column: • Fused Silica SP2560, 100 m *0,25 mm, 0,2 µm Film Fatty Acid Composition of Various Some Vegetable Oils Vegetable Oil C14:0 C16:0 C18:1 C18:2 C18:3 Olive Oil 10,67 74,08 6,92 <0,04 (7,5 - 20,0) (55,0 - 83,0) (3,5-21,0) <1 Pomace Oil 0,0 11,1 68,8 11,5 0,6 Hazelnut 0,0 5,1 79,9 10,0 0,2 High Oleic Rapeseed 0,0 3,3 69,4 16,4 2,2 HOSO 0,1 3,4 76,5 12,8 0,1 Almond Oil 0,0 5,8 63,6 23,8 0,4 Rapeseed Oil 0,0 4,4 60,0 18,4 8,0 Palmoil 1,0 42,5 37,9 9,2 0,0 Palmolein 1,0 38,7 41,4 11,3 0,1 Cotton Seed 0,6 21,3 16,8 54,6 0,3 Sesame Oil 0,0 9,0 38,1 43,2 1,1 Soyaoil 0,1 10,5 22,4 52,9 5,8 Rice Bran Oil 0,3 18,2 37,6 31,2 0,4 Corn Oil 0,0 10,3 30,3 53,9 0,7 Sunflower Oil 0,1 5,9 25,3 61,8 0,1 Safflower Oil 0,1 6,7 13,5 73,4 0,2 6 Triacylglycerol Patterns (GLC) of Some Vegetable Oils Vegetable Oil PLP POO PLO OOO OLO OLL LLL OOO/POO OLO/PLO OLL/LLL Olive Oil 0,9 22,8 5,4 40,6 9 1,3 0,1 1,75 1,58 13,00 Pomace Oil 1,4 20,5 7,7 32,3 12,3 2,8 0,5 1,58 1,60 5,60 Hazelnut 0,1 12,7 3,6 52,5 16,1 3,6 0,5 4,13 4,47 7,20 High Oleic Rapeseed 0,2 6,4 3,6 43,2 23,6 6,2 1,5 6,75 6,56 4,13 HOSO 0,1 8 1,7 55,9 8,1 4,6 3,1 6,99 4,76 1,48 Almond Oil 0,2 8,2 7,5 32,2 23,5 11,3 2,4 3,93 3,13 4,71 Rapeseed Oil 0,3 5,6 4,7 26,55 21,5 9,3 2,6 4,72 4,67 3,58 Palmoil 7,3 18,6 7,3 2,7 1,2 0,5 0,1 0,15 0,16 5,00 Palmolein 9,3 20,9 9,5 3,1 1,5 0,5 0,1 0,15 0,16 5,00 Cotton Seed 12,1 2,7 14 1 3,7 10,4 13,1 0,37 0,26 0,79 Sesame Oil 1,7 5,9 9,6 9,9 15,2 17,3 10 1,68 1,58 1,73 Soyaoil 2,9 3,2 10,4 3,1 8,2 17,5 19,3 0,97 0,79 0,91 Rice Bran Oil 6,4 10,8 16,5 7,5 12,1 9,9 4,1 0,69 0,73 2,41 Corn Oil 2,3 3,7 11,2 4,5 12,7 22,4 17,1 1,22 1,13 1,31 Sunflower Oil 1 1,7 6,45 3,55 10,25 26,4 23,6 2,19 1,65 1,12 Safflower Oil 1 1,1 4,8 1,8 3,65 16,9 43,25 1,64 0,76 0,39 DATA SET: Analysed Samples in 2004-2009 • Almond Oil 6 • Olive Oil 1980 • Apricot Oil 5 • Olive Oil (Pomace Oil) 15 • Argan Seed Oi 19 • Palm kernel 10 • Avocado(Pulp) Oil 5 • Palm oil 7 • Black Cumin Seed Oil 6 • Palm Olein 10 • Borage (Starflower) Oil 7 • Palmstearin 9 • Butterfat 40 • Pumpkin Seed Oil 13 • Cocoabutter 11 • Rape Seed Oil 139 • Coconut Oil 12 • Rape Seed Oil (High Oleic) 10 • Coconut Oil,hardened 4 • Saflower Seed Oil (High Oleic) 6 • Corn Oil 20 • Saflower Seed Oil (Linoleic) 23 • Cotton Seed Oil 6 • Sesame Oil 12 • Evening Primrose 5 • Sheep milk(fat) 12 • Goat's milk(Fat) 15 • Soybean 15 • Grape Seed Oil 16 • Sunflower Seed oil(High oleic)10 • Ground nut Oil 8 • Sunflower Seed oil(Linoleic) 70 • Hazelnut Oil 16 • Tallow(beef) 10 • Linseed Oil 17 • Walnut Oil 28 • Macadamia Oil 5 • Wheat Germ Oil 13 7 Data analysis Statistic Software: XLSTAT Version 2009.1.02, Copyright Addinsoft • K-Means and • Principal component analysis • Cluster analysis Principal Component Analysis Variablen (Achsen F1 und F2: 80,38 %) Variablen (Achsen F1 und F2: 50,80 %) 1 C16:0PLP 1 POP POO PLO 0,75 0,75 POP C18:1 C16:0 C16:1 0,5 0,5 C20:0 PLP OOO POO PLO C18:1(11c) C20:1 0,25 0,25 C18:3 C18:0 C22:0 OLO 0 0 C18:2 C10:0C12:0 LLL C14:0 -0,25 -0,25 F2 (33,76 %) OLL F2 (18,59 %) C18:1 -0,5 OOO OLO -0,5 C18:2OLL LLL -0,75 -0,75 -1 -1 -1 -0,75 -0,5 -0,25 0 0,25 0,5 0,75 1 -1 -0,75 -0,5 -0,25 0 0,25 0,5 0,75 1 F1 (46,62 %) F1 (32,21 %) 30 Objects 40 Objects 8 Principal Component Analysis F1 F2 Variable Variablen (Achsen F1 und F2: 80,38 %) C16:0 0,048 0,958 1 C16:0PLP C18:1 -0,920 -0,276 POP PLO 0,75 C18:2 0,940 -0,009 0,5 POP -0,344 0,873 POO 0,25 PLP 0,133 0,958 0 C18:2 POO -0,913 0,309 LLL -0,25 F2 %) (33,76 OLL PLO -0,122 0,740 C18:1 -0,5 OOO OLO OOO -0,884 -0,414 -0,75 -0,332 -0,421 OLO -1 OLL 0,785 -0,197 -1 -0,75 -0,5 -0,25 0 0,25 0,5 0,75 1 F1 (46,62 %) LLL 0,951 -0,101 Agglomatorative Hierachical Clustering Dendrogramm 0 0,1 0,2 0,3 0,4 0,5 0,6 Ähnlichkeit 0,7 0,8 0,9 1 9 Identification of an vegetable Oil using Excel (C16:0,C18:1,C18:2,POP,PLP,POO,OLO,OOO,LLL) Ea1, Eb1… Ea2, Eb2.. Ea3, Eb3 … (Ea1-Pa)2 /sdv(a)+ (Eb1-Pb) 2 /Sdv (b) Blends of Vegetable Oils with Identical Fatty Acid Compositions Olive Oil hoRP 40% hoSA 80% hoRP 5% hoSF hoSF 40% PO 20 % hoSF 75% PO 20 % PO 20 % C14:0 0 0.2 0.3 0.2 0.1 C16:0 10 12 11.8 11.8 5.5 C18:0 3 3.9 4.9 5.1 3.4 C18:1 77 68.3 72.8 72.2 76.5 C18:2 8 12.1 8 9.6 12.8 C18:3c 0.5 1.5 0.2 0.3 0.3 C20:0 0.5 0.5 0.5 0.4 0.2 Iodine 82 84.8 77 80 82 Value 10 Mathematical Procedure for the Identification of Olive Oils, Vegetable Oils and Blends • Reference Table with the data of olive oils, hazelnut, blends, vegetable oils, etc .
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