Mid-IR and Milk Chemistry
Lina Jonsson MSc Animal Science
Production Manager Miris AB,
Sweden
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Content
• What is Mid-IR?
-History about Mid-IR
-The principle of Mid-IR
-The advantage of Mid-IR
• How to make an accurate
calibration and take a correct
sample
• What is milk, what are we
measuring?
-Analytical methods for milk
• Human breast milk
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Gammarays
1 pm
X-rays
UV
VIS
IR
Micro-
Radio
waves
1 nm
1 um
NIR
1m
MIR
0.7 um
NITS
1 mm
2.5 um
NIRS
10
50 um
Liquid Transmission
MIR
2.5 um
700 nm 1100
10 um
2500 nm
Fat 3.5 5.7 Protein 6.5 Carbohydrate 9.5
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
History of Mid-IR
•
•
•
•
•
•
Liquid Transmission Spectroscopy
J.D.S Goulden 1961
IRMA
Interference Filters
FTIR
Solid-State
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Gammarays
1 pm
X-rays
UV
VIS
IR
Micro-
Radio
waves
1 nm
1 um
NIR
1m
MIR
0.7 um
NITS
1 mm
2.5 um
NIRS
10
50 um
Liquid Transmission
MIR
2.5 um
700 nm 1100
10 um
2500 nm
Fat 3.5 5.7 Protein 6.5 Carbohydrate 9.5
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Gammarays
1 pm
X-rays
UV
VIS
IR
Micro-
Radio
waves
1 nm
1 um
NIR
700 nm 1100
1m
MIR
0.7 um
NITS
1 mm
2.5 um
10
50 um
NIRS
2500 nm
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Milk Spectra
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Principles of Mid-IR
IR source Cuvette WavebandDetector CPU
Selector
Beräknings
enhet
Energy
Energy
Wavelength
Energy
Wavelength
Wavelength
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Milk Spectra
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Milk Determination mid-IR
Milk
Water
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Milk Determination mid-IR
Milk
Water
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Spectra Milk
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Milk vs Milkfat
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Infrared Spectroscopy
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Infrared Spectroscopy
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Spectra of Milk and Skimmilk
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Milk vs Milkprotein
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Infrared Spectroscopy
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Milk vs Lactose
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Infrared Spectroscopy
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
The advantages of Mid-IR
• Quick analytical result
• The milk can be used after the
composition is known
• The composition of fat protein and
lactose in the same analyse
• Identify dilution before the milk has
entered the manufacture
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
How to make an accurate calibration and take a
correct sample
•
•
•
•
A certified reference lab
High quality of the milk
Homogenous milk
Good sampling routines
imperative to obtain
representative samples
• All result must be review
critical, mistakes do happen
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Sampling
Inhomogenity of milk demands special treatments of
milk before sampling and/or analyse
-Creaming
-Aggregation
-Foaming
Protein Chain
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Heating/Mixing
• Mixing more effective of warm
samples (40-43 C)
• Fat aggregations are dissolved.
• Condensed water is mixed into
the milk
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Ultrasound Treatment
• Previously frozen milk ought to be
treated ultrasound
• 1 second / ml
• The efficiency of treatment is increased
by temp. 40°C is optimal for milk
• Protein aggregation are dissolved
• Oil droplets are emulsified
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Chemical/Physical factors that interferes with
the “true” value of the milk
• Non Protein Nitrogen (NPN)
• Lactic acid
• Lipolysis
• Free fatty acids
• Creaming
• Oiling off
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
”Oiling off”
+
BAD MILK
GOOD MILK
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Fat globule (schematic)
Lipophile part
Phospholipids
+ membrane
Hydrophile part
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
What is milk , what are we measuring?
What is milk according to
definition???
Milk fat
Milk protein
Lactose
Dry matter (Total solids)
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Analytical Methods for Milk
Cow Milk
– Different international standards (ISO/IDF/AOAC)
for measuring constituents in milk. Also valid for
other species.
– (ISO 9622:1999; ISO 1211; ISO 8968-1 etc)
Human Milk
No international standards for human milk
methods.
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Analytical Methods
Fat
•
•
•
•
•
•
Gerber, Babcock, Lindström
Röse-Gottlieb, Mojonnier
Turbimetric (Milko-Tester)
MIR (Mid Infrared Transmission)
NIR (Near Infrared Reflectance/Transmission)
Ultrasonic high frequency
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Analytical Methods
Protein
•
•
•
•
Kjeldahl
MIR Mid Infrared Transmission
NIR Near Infrared Transmission/Reflectance
(Ultrasonic high frequency)
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Analytical Methods
Lactose
•
•
•
•
•
•
Luff-Schoorl
HPLC
Enzymatic
MIR Mid Infrared Transmission
(NIR)
(Ultrasonic)
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Analytical Methods
• IDF recommended methods
•
•
•
•
Röse-Gottlieb
Kjeldahl
Enzymatic
Drying oven 102°C
Milk fat
Milk protein
Lactose
Dry matter
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Analytical Metods
Röse-Gottlieb
•
•
•
•
•
Neutral glycerider
FFA
Phospholipids
Sterols
Others (fat soluble vitamins.)
%
98.7
0.1
0.8
0.3
0.1
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Analytical Methods
Kjeldahl
Protein-N
NPN-N
Total-N
Cow
%
% of milk
95
3.04
5
0.16
100 3.20
Human
%
75
25
100
% of milk
0.9
0.3
1.2
Urea-N, Creatine-N, Uric-N, Peptide-N,
Ammonia-N
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Analytical Methods
Enzymatic
• Water accounts about
• Lactose monohydrate
• Lactose anhydrous
5%
5.00 %-units
4.75 %-units
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Analytical Methods
Drying oven
• All that evaporate is measured as water
• Volatile components (Lactic acid, fatty acids, CO2, NH3 )
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Human breast milk
•
•
•
•
Unsaturated fat
Day to day variation
Protein composition
Lactose
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Fatty Acid
4:0
6:0
8:0
10:0
12:0
14:0
15:0
16:0
16:1
17:0
18:0
18:1
18:2
CLA
18:3
Cow
4.0
2.6
1.4
3.1
3.3
10.6
0.9
27.7
0.9
0.5
8.2
15.4
2.4
0.47
0.8
(% wt/wt)
Human
1.3
3.1
5.1
0.4
20.2
5.7
Rat
1.1
7.0
7.5
8.2
5.9
36.4
13.0
22.6
1.9
0.3
6.5
26.7
16.3
1.4
0.8
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Human breast milk
Day to day variation
S. Polberger and B. Selander, 2007.
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Protein
Casein
α-casein
β-casein
Whey
κ-casein
βlactoglobulin
αlactalbumin
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Protein
Casein
β-casein
Whey
κ-casein
Lactoferrin
αlactalbumin
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Analytical Methods
Oligosaccharides
Three to ten monosaccharides including glucose, galactose,
fucose, sialic acid, N-acetylglucoseamine
Account for about 0.8-1.2 g/100 ml
Complicated analytical methods, but mid-infrared methods
seems to measure this carbohydrates due to hydroxyl (-OH)
groups
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Summary
• Milk is not a solution, it is a emulsion. The different
components can aggregate or separate, which makes
sampling difficult.
• The Mid-IR method only need one sample to give the
complete major components of milk
• This reduce the source of error and makes the result more
comparable
• A small amount of milk is needed, the result comes with in a
minute
• No chemicals is needed
• Approved by IDF
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Questions?
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se
Thanks for
the attention!
Miris AB | Kungsgatan 11, 753 18 Uppsala, Sweden | tel: +46 18 146 907 | www.miris.se