Milk Fat Adulteration Testing

Elena Grishina

15th of Oct 2015

CUSTOMER DAY

MOSCOW 2015

CUSTOMER DAY

MOSCOW 2015

1. Why milk fat adulteration tests are important ?

2. Evolution of milk fat adulteration tests

3. Fatty acids testing

4. Example of fatty acids of milk fat and palm oil blends

5. Typical milk fat adulteration tests in Russia

6. Future of milk fat adulteration tests

7. Summary

Agenda :

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MOSCOW 2015

Why milk fat adulteration tests are important ?

Does your company faces the problem of adulteration of

the dairy products?

What do you estimate the percentage of adulterated

products?

50% canned sweet

milk

30% butter

25% curd and

sour cream

20% cheeses

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Why milk fat adulteration tests are important ?

Let’s discuss how these figures were calculated …

50% canned sweet

milk

30% butter

25% curd and

sour cream

20% cheeses

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Evolution of milk fat adulteration tests

FAME

(fatty-acids

composition test)

Determination of milk

fat purity by gas

chromatographic

analysis of sterols

GOST 33490 – 2015

Determination of milk

fat purity by gas

chromatographic

analysis of

triglycerides

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Fatty acid testing

The fatty acid composition of milk fat varies due to a large number of factors, including: • Genetic variation in the dairy herd • Breed of cow • The stage of lactation of the cow • The composition of the diet of the cow, including variations in pasture due to climatic conditions, and supplementary feeding regimes. These factors result in variations throughout the dairy season, between seasons, and from region to region. In particular, differences in farming practices such as year-round calving versus spring calving and different feeding regimes mean that there are large differences in the fatty acid composition of milk fat produced in different countries or different regions of country. These differences can change with time as feeding and farming practices change and so then typical ranges need to be constantly updated.

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Fatty acid testing Table 1: Fatty acid content of a range of palm oil / milkfat blends (% of palm oil in milkfat)

0% 10% 20% 30% 40% 50% 100%

C4:0 3.3 3 2.6 2.3 2 1.6 0

C6:0 2.2 1.9 1.7 1.5 1.3 1 0

C8:0 1.4 1.2 1.1 0.9 0.8 0.7 0

C10:0 3.3 3 2.6 2.3 2 1.6 0

C10:1 0.3 0.3 0.3 0.2 0.2 0.2 0

C12:0 4.5 4.1 3.7 3.2 2.8 2.4 0.4

C14:0 12.6 11.4 10.2 9 7.9 6.7 1.1

C14:1 1 0.9 0.8 0.7 0.6 0.5 0

C15:0 1.3 1.2 1 0.9 0.8 0.6 0

C16:0 31.1 32.5 34.1 35.3 36.8 38 44.3

C16:1 1.7 1.5 1.3 1.2 1 0.9 0.2

C17:0 0.5 0.5 0.4 0.4 0.3 0.3 0.1

C17:1 0.3 0.3 0.2 0.2 0.2 0.2 0

C18:0 9.1 8.7 8.1 7.7 7.2 6.7 4.4

C18:1 19.7 21.8 23.9 25.9 27.9 29.9 39.4

C18:2 1.2 2.1 2.9 3.8 4.5 5.4 9.3

C18:2 1.3 1.2 1 0.9 0.7 0.6 0

C18:3 0.7 0.6 0.6 0.5 0.5 0.4 0.2

Obviously adding more palm oil results in a fatty acid content which

approaches that of pure palm oil (as highlighted, the C12:0 decreases

and the C16:0 and C18:1 increase)

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Example of fatty acids of milk fat and palm oil blends

FAME ratio 0% 10% 20% 30% 40% 50% 100%

GOST 32261-2013 for butter the

Customs Union origin

GOST 32261-2013 for butter New Zealand origin

Low high Low high

C16:0/C12:0 6.9 7.9 9.2 11.0 13.1 15.8 110.8 5.8 14.5 5 14.5

C18:0/C12:0 2.0 2.1 2.2 2.4 2.6 2.8 11.0 1.9 5.9 1.7 5.9

C18:1/C14:0 1.6 1.9 2.3 2.9 3.5 4.5 35.8 1.6 3.6 1.5 3.6

C18:2/C14:0 0.2 0.3 0.4 0.5 0.7 0.9 8.5 0.1 0.5 0.1 0.5

unsat/sat 0.4 0.4 0.5 0.6 0.6 0.7 1.0 0.4 0.7 0.4 0.7

Note Unsat/sat is the ratio of specific fatty acids from these groups

unsat/sat = Sum of C18:1+C18:2 vs Sum C12:0+C14:0+C16:0+C18:0

Table 2: Fatty acid content of a range of palm oil / milk fat blends (% of palm oil in milk fat)

Current FAME test is not a sensitive enough to define 40% of palm oil in milk fat.

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Example of fatty acids of milk fat and palm oil blends

Current FAME test is not a sensitive enough to define 40% of palm oil in milk fat.

Too expensive mistake …

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Typical milk fat adulteration tests in Russia

- not sensitive enough

- Not applicable for all dairy products

- not all labs are able to complete properly

+ very common

+ all Controlling Authorities ( e.g. Rospotrebnadzor) are used to use

FAME

95% - not very known

- interpretation part needs to be improved

- not all labs have accreditation

+ very sensitive

+ can be used for all dairy products

+ reference method

Plant sterols

5%

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Future of milk fat adulteration tests

accu

racy

Fatty acid composition test

Plant sterol test Chromatographic analysis of

triglycerides

Current 2015-2016 2016..

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Summary :

• Milk fat adulteration testing is important for the pure identity of dairy products

• Fatty acid (FAME) testing, which simply identifies the fatty acids, is not a sensitive test

• Testing for excess plant sterols in the product is more sensitive for the detection of vegetable oil contaminants

• The recent ISO IDF triglyceride s-value method is much more sensitive than the fatty acid tests because it analyses how the fatty acids are assembled into the triglyceride