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Dr Rodney Mailer - Australian Oils Research Australia 1 American Oil Chemists’ Society Australasian Section Adulteration of Olive Oil Rod Mailer & Jamie Ayton 9-11 September 2015 The Pier, Geelong, Victoria AUSTRALIA

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Dr Rodney Mailer - Australian Oils Research Australia

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American Oil Chemists’ Society

Australasian Section

Adulteration of Olive Oil

Rod Mailer & Jamie Ayton9-11 September 2015

The Pier, Geelong, Victoria

AUSTRALIA

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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.

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BIJU ANTONY, Chief Librarian, NDRK College of Nursing, BM Road, Hassan, Karnataka, India

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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.

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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.

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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…

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Adulteration Fraud

Seed Oils

Refined Oils

Pomace Oils

Aged Oils

Poor Storage

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73% (60) of imported

oils failed sensory test

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UC Davis Study

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SENSORY IOC CHEMICAL TESTDGF / Aust

Tests

BRANDFAILED

SENSORYFFA FAP PV UV DAGs PPP

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

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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)

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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

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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

C18:2T and C18:3T 0.04 < 0.05Stigmasta-3,5-diene from dehydration of B-sitosterol

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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

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Harvesting

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ppnt.pdfppnt2.pdf

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Temperature & Humidity in Ocean ContainersDavid 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.

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Figure 7: Hottest Shipment 135 F [57 C]

Japan to Memphis

140

120 Temperature53

Relative Humidity43

100

33

8023

6013

40 3

20

04-Jul-05

-7

09-Jul-05 14-Jul-05

Date

19-Jul-05 24-Jul-05

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.

Extreme conditions in Ocean Containers

Ocean Container Temperature and Humidity Study David A. Leinberger, 2/27/2006

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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

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Grades of Olive Oil

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IOC Codex EU Australia COOC USA

Extra virgin olive oil ✔ ✔ ✔ ✔ US ✔

Virgin olive oil ✔ ✔ ✔ ✔ US ✔

Ordinary virgin olive oil ✔ X X X X

Lampante virgin olive oil X Lampante olive oil ✔ Crude olive oilUS VOO not fit for

human consumption

Refined olive oil ✔ ✔ ✔ ✔ US ✔

Olive oil ✔Olive oil composed of

ROO and VOOOlive oil-composed of

ROO and VOOROO blend composed

of ROO and VOOUS ✔

Crude olive-pomace oil X ✔ ✔ ✔ US ✔

Refined olive-pomace oil ✔ ✔ ✔ ✔ US ✔

Olive-pomace oil ✔ ✔OPO composed of RO-

PO and VOO

RO-PO blend composed of RO-PO

oil & VOO

US ✔

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Fatty Acid Profiles in Olive Oil

Fatty acid (%m/m methyl esters)

IOC Codex EU Australia COOC USA

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 ✔ ✔ ✔ ✔ ✔

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Pyropheophytin - PPP(Lit. K.Aizetmüller, Fett/Lipid 1986)

Chlorophyll a

H2O, 100 °C

Chlorophyll a‘

-Mg++

Pheophytin a‘

Pyropheophytin a

> 100 °C

Pheophytin a

Pyrochlorophyll a

> 100 °C

> 100 °C

-Mg++

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Pyropheophytin a

Pyropheophytin a

Not heated

160°C 60 min

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Pyropheophytin a – (Temperature)

Low PP, High C18:2

Months

0 3 6 9 12 15 18 21 24 27 30 33 36

% p

yro

pheophytin a

0

10

20

30

40

50

60

70

80

90

100

Mid PP, Mid C18:2

Months

0 3 6 9 12 15 18 21 24 27 30 33 36

15oC, dark, closed

22oC, dark, closed

37oC, dark, closed

High PP, Low C18:2

Months

0 3 6 9 12 15 18 21 24 27 30 33 36

Least stable Most stable

AS-5264-2011 – < 17%•Age

•Temperature

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1,2-Diacylglycerides

Formation of diacylglycerides

1,2-Diacylglyceride 1,3-Diacylglyceride

Temperature, TimeCourtesy Boundary Bend

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Effect of storage temperatures

3 olive oils over 36 months

a) LP,HL

% 1

,2-d

iacylg

lycero

ls

0

10

20

30

40

50

60

70

80

b) MP,ML

%1,2

-dia

cylg

lycero

ls

0

10

20

30

40

50

60

70

80

c) HP,LL

Months

0 3 6 9 12 15 18 21 24 27 30 33 36

%1,2

-dia

cylg

lycero

ls

0

10

20

30

40

50

60

70

80

15oC, dark, closed

22oC, dark, closed

37oC, dark, closed

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1,2 Diacylglyceride

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Sensory AnalysisLow PP, High C18:2

Storage (months)

0 3 6

Org

anole

ptic s

core

0

1

2

3

4

5

6

7

High PP, Low C18:2

Storage (months)

0 3 6

Org

anole

ptic s

core

0

1

2

3

4

5

6

7

15oC, dark, nil O2

22oC, dark, nil O2

37oC, dark, nil O2

Light, 22oC, nil O2

oxygen, dark, 22oC

Fruitiness

Defects

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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.

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Summary

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Adulteration - Fraud

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Fatty Acid Profiles – Other oils

Fatty acid IOC Olive oilCodex - Mid Oleic

Sunflower oilCodex - High OleicSafflower 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

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Fatty acid Profile - Canola oil

Fatty acid IOC Olive oilHigh Oleic

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

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* Dow Agrosciences