1 American Oil Chemists’ Society Australasian Section
Adulteration of Olive Oil
Rod Mailer & Jamie Ayton 9-11 September 2015 The Pier, Geelong, Victoria AUSTRALIA
Dr Rodney Mailer - Australian Oils Research Australia 2 Adulteration
Adulteration: addition of another substance to a food item in order to increase the quantity of the food item, which may result in the loss of quality of food item.
Dr Rodney Mailer - Australian Oils Research Australia 3
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BIJU ANTONY, Chief Librarian, NDRK College of Nursing, BM Road, Hassan, Karnataka, India Dr Rodney Mailer - Australian Oils Research Australia 4 Adulteration
Argemone “mexicana” oil in adulterated mustard oil can cause a condition similar to epidemic dropsy which can be fatal
Adulterated rapeseed oil in Spain in 1981: toxic oil syndrome affecting 25,000 people. A multisystemic disease caused about 600 deaths and 300 invalids. Nothing is yet known about the nature of the causative agent
Chinese milk scandal 2008: milk and infant formula adulterated with melamine - an estimated 300,000 victims, 6 infants dying from kidney damage and 54,000 babies being hospitalised.
Cattle Feed: mustard substituted for canola meal.
Dr Rodney Mailer - Australian Oils Research Australia 5 EU Report A7-0434/2013:
Top 10 products most at risk of food fraud
1. Olive oil 2. Fish 3. Organic foods 4. Milk 5. Grains 6. Honey and maple syrup 7. Coffee and tea 8. Spices (such as saffron and chili) 9. Wine 10. Certain fruit juices
Defining the Public Health Threat of Food Fraud / Spink, J, and Moyer,: Journal of Food Science, 2011, Volume 75 (Number 9), p. 57-63. 6
Slippery Business – The New Yorker AUG 6, 2007
BY TOM MUELLER
On August 10, 1991, a rusty tanker called the Mazal II docked at the industrial port of Ordu, in Turkey, and pumped twenty-two hundred tons of hazelnut oil into its hold…
Dr Rodney Mailer - Australian Oils Research Australia 7 Adulteration Fraud
Seed Oils
Refined Oils
Pomace Oils
Aged Oils
Poor Storage
Dr Rodney Mailer - Australian Oils Research Australia 73% (60) of imported oils failed sensory test UC Davis Study
DGF / Aust SENSORY IOC CHEMICAL TEST Tests
FAILED BRAND FFA FAP PV UV DAGs PPP SENSORY
California Olive Ranch 0 0 0 0 0 0 0 Cobram Estate 0 0 0 0 0 0 0 Lucini 11 0 0 0 100 0 0 Filippo Berio 83 0 0 0 33 33 20 Star 61 0 0 0 0 64 27 Bertolli 72 0 0 0 8 62 46 Colavita 56 0 0 0 50 70 50 Pompeian 94 0 0 0 65 100 94 Failed (%) 51% 0 0 0 34 65 49 9 Australian Olive Association Routine Market Surveys September 2011 and April 2015
331 oils from supermarkets/retail outlets WA, SA, Vic and NSW.
Australian brands 105/160 (66%) Imported brands 53/171 (31%)
Total 158/331 (48%)
Australian Standards for Olive Oil and Olive-Pomace Oil AS5265-2011 (AS) IOC Tests Results IOC limits
Free Fatty Acids 0.27 < 0.8 Peroxide Value 17 < 20 UV Absorbance ∆K 0.070 < 0.01 K232nm 3.188 < 2.50 K270nm 0.892 < 0.22 Stigmastadiene Content 6.160 < 0.10 Wax Content 2002 < 250 Trans Fatty Acids C18:1T 0.071 < 0.05 C18:2T and C18:3T 0.099 < 0.05 IOC Tests Results IOC limits
Free Fatty Acids 0.19 < 0.8 Peroxide Value 4 < 20 UV Absorbance ∆K 0.026 < 0.01 K232nm 1.98 < 2.50 K270nm 0.34 < 0.22 Stigmastadiene Content 14.49 < 0.10 Wax Content 196 < 250 Trans Fatty Acids C18:1T 0.03 < 0.05 Stigmasta-3,5-diene from dehydration of B-sitosterol C18:2T and C18:3T 0.04 < 0.05 IOC Tests Results IOC limits
Free Fatty Acids 0.56 < 0.8 Peroxide Value 7 < 20 UV Absorbance ∆K 0.003 < 0.01 K232nm 1.88 < 2.50 K270nm 0.12 < 0.22 Pyropheophytin a 31.5 <17* 1,2-diacylglycerols 29.8 >35* Sensory analysis Defect - rancid 1.5 0 Harvesting
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ppnt.pdf ppnt2.pdf 17
Temperature & Humidity in Ocean Containers David Leinberger, Senior Packaging Engineer, Xerox Corporation, Wilsonville, USA
One year study of ocean container temperature and humidity for shipments between Asia, Europe and North America.
Dr Rodney Mailer - Australian Oils Research Australia 18
Extreme conditions in Ocean Containers Stage 1. Filling, loading onto ship, road transportation and brief periods of storage. Daily cycles of temperature and humidity are common
Stage 2. Time at sea or aboard a ship. - extreme conditions are rare
Stage 3. Container removed from the ship until the unloading process. Daily temperature and humidity cycles are common and may be extreme.
Figure 7: Hottest Shipment 135 F [57 C] Japan to Memphis 140 53 120 Temperature Relative Humidity 43 100 33 80 23
60 13
40 3
20 -7 04-Jul-05 09-Jul-05 14-Jul-05 19-Jul-05 24-Jul-05 Date
Ocean Container Temperature and Humidity Study David A. Leinberger, 2/27/2006 19
International Olive Council
Madrid Spain 1959 formed under auspices of United Nations
Most national standards based on IOC Standards
9 Grades of Olive oil
Test ~50 components of olive oil
Limits are based on southern European climates
Dr Rodney Mailer - Australian Oils Research Australia 20 Grades of Olive Oil
IOC Codex EU Australia COOC USA
Extra virgin olive oil ✔ ✔ ✔ ✔ US ✔
Virgin olive oil ✔ ✔ ✔ ✔ US ✔
Ordinary virgin olive oil ✔ X X X X
US VOO not fit for Lampante virgin olive oil Lampante olive oil ✔ Crude olive oil X human consumption
Refined olive oil ✔ ✔ ✔ ✔ US ✔
Olive oil composed of Olive oil-composed of ROO blend composed Olive oil ✔ US ✔ ROO and VOO ROO and VOO of ROO and VOO
Crude olive-pomace oil X ✔ ✔ ✔ US ✔
Refined olive-pomace oil ✔ ✔ ✔ ✔ US ✔
RO-PO blend OPO composed of RO- US ✔ Olive-pomace oil ✔ ✔ composed of RO-PO PO and VOO oil & VOO
Dr Rodney Mailer - Australian Oils Research Australia 21
Fatty Acid Profiles in Olive Oil
Fatty acid (%m/m IOC Codex EU Australia COOC USA methyl esters) Myristic acid < 0.03 < 0.05 < 0.05 < 0.05 < 0.05 < 0.05 Palmitic acid 7.5 - 20.0 ✔ ✔ 7.0 - 20.0 7.0 - 22.0 ✔ Palmitoleic acid 0.3 - 3.5 ✔ ✔ ✔ 0.25 - 3.5 ✔ Heptadecanoic < 0.3 ✔ ✔ ✔ ✔ ✔ Heptadecenoic < 0.3 ✔ ✔ < 0.4 < 0.5 ✔ Stearic acid 0.5 - 5.0 ✔ ✔ ✔ ✔ ✔ Oleic acid 55.0 - 83.0 ✔ ✔ 53.0 - 85.0 50.0 - 85.0 ✔ Linoleic acid 3.5 - 21.0 ✔ ✔ 2.5 - 22.0 2.5 - 22.0 ✔ Linolenic acid < 1.0 ✔ < 1.5 < 1.5 < 1.5 Arachidic acid < 0.6 ✔ ✔ ✔ ✔ ✔ Gadoleic acid < 0.4 ✔ ✔ < 0.5 < 0.5 ✔ Behenic acid < 0.2* ✔ ✔ ✔ ✔ ✔ Lignoceric acid < 0.2 ✔ ✔ ✔ ✔ ✔
Dr Rodney Mailer - Australian Oils Research Australia Pyropheophytin - PPP (Lit. K.Aizetmüller, Fett/Lipid 1986)
Chlorophyll a
H O, 100 C 2 ° > 100 °C
Chlorophyll a‘ Pyrochlorophyll a Pheophytin a -Mg++ -Mg++ Pheophytin a‘ > 100 °C > 100 °C
Pyropheophytin a Pyropheophytin a
Not heated
Pyropheophytin a
160°C 60 min Pyropheophytin a – (Temperature)
Low PP, High C18:2 Mid PP, Mid C18:2 High PP, Low C18:2 Least stable Most stable 100 90 80 70 60 50 40 30 % pyropheophytin a pyropheophytin % 20 10 0 0 3 6 9 12 15 18 21 24 27 30 33 36 0 3 6 9 12 15 18 21 24 27 30 33 36 0 3 6 9 12 15 18 21 24 27 30 33 36
Months Months Months
15oC, dark, closed 22oC, dark, closed 37oC, dark, closed •Age AS-5264-2011 – < 17% •Temperature 1,2-Diacylglycerides
Formation of diacylglycerides
1,2-Diacylglyceride 1,3-Diacylglyceride
Temperature, Time Courtesy Boundary Bend 26
80 15oC, dark, closed a) LP,HL 22oC, dark, closed 70 37oC, dark, closed
60 1,2 Diacylglyceride 50 40
30
% 1,2-diacylglycerols 20
10
0
80 b) MP,ML
70
60
50
40
30
Effect of storage temperatures %1,2-diacylglycerols 20
10
3 olive oils over 36 months 0 80 c) HP,LL
70
60
50
40
30
%1,2-diacylglycerols 20
10
0
0 3 6 9 12 15 18 21 24 27 30 33 36
Months High PP, Low C18:2
7
6
5
4
3
2
Organoleptic score Organoleptic
1
0
0 3 6 Storage (months)
15oC, dark, nil O Sensory Analysis 2 Low PP, High C18:2 o 22 C, dark, nil O2 o 7 37 C, dark, nil O2 o 6 Light, 22 C, nil O2 oxygen, dark, 22oC 5
4
3 Fruitiness
2
Organoleptic score Organoleptic
1 Defects 0
0 3 6 Storage (months) 28 Extent of Fraud
US International Trade Commission, 2012 - olive oil authenticity. Washington DC, USA
European Union Workshop on Adulteration in Olive Oil, 2013 – oil testing/fraud/ authenticity, Madrid
Codex Alimentarius – 2013 Codex Alimentarius Fats and Oils, Langkawi, Malaysia Codex Alimentarius – 2015 Codex Alimentarius Fats and Oils, Malacca, Malaysia
ISO Fats and Oils – 2014 ISO TC 34; Berlin, Germany ISO Fats and Oils – 2015 ISO TC 34; Gouda, Netherlands
Californian Olive Oil Commission – 2014 - new trading standard for olive oil in California
Multiple Legal Cases, USA – 2010-2015 – Washington, New York, San Francisco, Sydney, Adelaide.
Dr Rodney Mailer - Australian Oils Research Australia 29 Summary
Dr Rodney Mailer - Australian Oils Research Australia 30 Adulteration - Fraud
Dr Rodney Mailer Australian Oils Research Australia 31
Fatty Acid Profiles – Other oils
Codex - Mid Oleic Codex - High Oleic Fatty acid IOC Olive oil Sunflower oil Safflower seed Oil Myristic acid < 0.03 ND-0.1 ND - 0.2 Palmitic acid 7.50 - 20.00 2.6-5.0 3.6 - 6.0 Palmitoleic acid 0.30 - 3.50 ND-0.1 ND - 0.2 Heptadecanoic < 0.03 ND-0.1 ND - 0.1 Heptadecenoic < 0.03 ND-0.1 ND - 0.1 Stearic acid 0.50 - 5.00 2.9-6.2 1.5 - 2.4 Oleic acid 55.00 - 83.00 75 - 90.7 70.0 - 83.7 Linoleic acid 3.50 - 21.00 2.1 - 17.0 9.0 - 19.9 Linolenic acid < 1.00 ND - 0.3 ND - 1.2 Arachidic acid < 0.60 0.2 - 0.5 0.3 - 0.6 Gadoleic acid < 0.40 0.1 - 0.5 0.1 - 0.5 Behenic acid < 0.20* 0.5 - 1.6 ND - 0.4 Lignoceric acid < 0.2 ND-0.5 ND - 0.3
Dr Rodney Mailer - Australian Oils Research Australia 32 Fatty acid Profile - Canola oil
High Oleic Fatty acid IOC Olive oil Canola (Rapeseed) Oil* Myristic acid < 0.03 Palmitic acid 7.50 - 20.00 7 Palmitoleic acid 0.30 - 3.50 Heptadecanoic < 0.03 Heptadecenoic < 0.03 Stearic acid 0.50 - 5.00 Oleic acid 55.00 - 83.00 73 Linoleic acid 3.50 - 21.00 15 Linolenic acid < 1.00 <3 Arachidic acid < 0.60 Gadoleic acid < 0.40 Behenic acid < 0.20* Lignoceric acid < 0.2
* Dow Agrosciences Dr Rodney Mailer - Australian Oils Research Australia