nutritional metrology: the role of reference materials in improving quality of fats and oils...
DESCRIPTION
Oils & Fats Presentation By: Dr. Dr. Ibrahim TahounTRANSCRIPT
Nutritional Metrology: The Role of Reference
Materials in Improving Quality of
Fats and Oils Analysis
Dr. Ibrahim Tahoun
National Institute of Standards
Mobile: 01002644877
1
Metrology = science of measurement
and its applications
2
Metrology Applications
Reference Materials (Preparation and Use)
Traceability and Calibration in Chemical
Measurements
Validation of Measurement Procedures
Uncertainty of Measurement Results
Statistical Treatments of Analytical Results
Quality Assurance [Internal& External]
3
Data Quality
Organizational structure
Management system
Quality manual
Document control
Qualified and trained
staff
Documented and validated
method
Calibrated and
maintained instrument
(Certified) reference material
Quality Control
PT
Quality of Measurement Results
Measurement results must be:-
Traceable to a known and recognizable set of
national and international standards.
Valid and accurate measurements depend upon
use of valid methods of analysis and use of
reference materials and establishment of adequate
quality control systems.
5
Traceability to SI Units
Traceability to the International System of Units (SI) leads to
measurement results that have three properties.
Stable
Results from measurements of the same quantity against the
same reference in one laboratory will be stable over time.
Comparable
Results from measurements of the same quantity against the
same reference in different laboratories will be comparable over
both time and space.
Absolute
Results from measurements of the same quantity against
different references will be same over both time and space.
International traceability to the SI provides all three of these
6
Reference materials Laboratory is primary metrology
laboratory (Metrology in Chemistry), it develops national
measurement standards (CRM).
Development and improvement of certification, harmonization
and compatibility of reference materials with international
standards.
Technical support to industry in everything related to
measurements, reference materials and data to establish
traceability of their measurements.
Traceability to SI Units
Traceability to SI Units
Traceability to SI Units
NIS
AWA
EGAC
EOS
Traceability to SI Units
Reference Materials
RM Laboratory Produced number of Reference materials for
food analysis:-
- Anions standard solutions
- Elemental standard solutions
- Pesticides solutions
- Vitamins in Milk Powder and Infant Formula
- Tocopherols in Edible oils
13
RM Production
Different indicator parameters are used to assess the quality of
edible fats and oils, including:-
Iodine value
Free, trans fatty acids and fatty acids profile
Heavy metals and trace elements and phosphorus content
Tocopherol and tocotrienol contents
Mono-, di-, triglyceride contents
Residual solvents
Water content
Quality of Edible Fats and Oils
Individual and total sterols contents
Saponification value
Peroxide value
Acid value and acidity
Ester value
Turbidity
Color
Flash and smoke point
Refractive index
Quality of Edible Fats and Oils
Test Method Equipment
Determination of heavy metals and trace elements BS EN ISO 5774:2001 AAS
Determination of phosphorus content BS ISO 10540-2:2003
Determination of benzo[a]pyrene ISO15302:2010 HPLC
Determination of stigmastadienes in vegetable oils BS EN ISO 15788-2:2004
Determination of tocopherol and tocotrienol contents BS EN ISO 9936:2006
Determination of residual benzene content BS ISO 14714:1998 GC and GC-MS
Determination of free and total glycerol and mono-, di-, triglyceride contents EN 14105
Determination of individual and total sterols contents BS EN ISO 2228:1999
Determination of aliphatic alcohols content BS ISO 12871:2010
Determination of total residual hexane BS EN ISO 8892:1995
Determination of water content BS ISO 11021:1999 KF
Determination of iodine value BS EN ISO 961:2000
Determination of moisture and volatile matter content BS 4325-1: 1978
Determination of saponification value BS EN ISO 657:2003
Determination of peroxide value ISO3960:2007
Determination of acid value and acidity ISO 660:2009
Determination of acid value BS ISO 1242:1999
Determination of ester value BS ISO 709:2001
Determination of Turbidity Turbidity meter
Determination of Color Lovibond
Determination of Flash and smoke point
Determination of refractive index Refractometer
min15 20 25 30 35 40 45 50 55
mAU
0
2
4
6
8
10
12
DAD1 C, Sig=298,8 Ref=360,16, TT (TOCOPHEROL 24-9-2012\TOCO 2012-09-25 11-19-15\012-0201.D)
β -
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γ -
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ph
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β -
toco
ph
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l
α-t
oco
ph
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Vitamin E Isomers in Corn Oil by Normal and
Reversed Phase Liquid Chromatography
m in6 8 1 0 1 2 1 4
mAU
0
2
4
6
8
1 0
1 2
1 4
D A D 1 C , S ig = 2 9 8 ,8 R e f= o ff (T O C O N P \P A R A B E N S 2 0 1 3 -0 1 -0 1 1 0 -4 6 -0 3 \0 8 1 -0 1 0 1 .D )
5.6
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7.5
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8.8
34
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δ-t
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10
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min20 30 40 50
mAU
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1
2
3
4
5
6
7
DAD1 C, Sig=298,8 Ref=360,16, TT (TOCOPHEROL 24-9-2012\TOCO 2012-09-25 11-19-15\011-0101.D)
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Vitamin E Isomers in Peanut Oil by Normal and
Reversed Phase Liquid Chromatography
m in6 8 1 0 1 2 1 4
mAU
0
2
4
6
8
1 0
1 2
1 4
D A D 1 C , S ig = 2 9 8 ,8 R e f= o ff (T O C O N P \P A R A B E N S 2 0 1 3 -0 1 -0 1 1 3 -4 5 -5 4 \0 8 2 -0 2 0 1 .D )
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δ-t
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min20 30 40 50
mAU
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2.5
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3.5
DAD1 C, Sig=298,8 Ref=360,16, TT (TOCOPHEROL 24-9-2012\TOCO 2012-09-24 12-37-09\002-0201.D)
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Vitamin E Isomers in Soybean Oil by Normal and
Reversed Phase Liquid Chromatography
m in6 8 1 0 1 2 1 4
mAU
0
2
4
6
8
1 0
1 2
1 4
D A D 1 C , S ig = 2 9 8 ,8 R e f= o ff (T O C O N P \P A R A B E N S 2 0 1 3 -0 1 -0 1 1 3 -4 5 -5 4 \0 8 3 -0 3 0 1 .D )
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min0 2.5 5 7.5 10 12.5 15 17.5
mAU
0
50
100
150
200
DAD1 A, Sig=325,8 Ref=off (W SV 2012\NP\SIG1000072.D)
3.8
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Fat Soluble Vitamin in Infant Formula by Normal and
Reversed Phase Liquid Chromatography
Fat Soluble Vitamin in Milk Powder by Normal and
Reversed Phase Liquid Chromatography
min4 6 8 10 12 14 16 18
mAU
0
50
100
150
200
250
DAD1 C, Sig=296,8 Ref=off (WSV 2012\SIG1000077.D)
4.6
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min0 2.5 5 7.5 10 12.5 15 17.5
mAU
0
50
100
150
200
250
DAD1 B, Sig=296,8 Ref=off (W SV 2012\NP\SIG1000067.D)
3.6
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6
Fatty acid Composition by Gas Chromatography
Equipment and Facilities
- Gas Chromatography with variety of detectors (ECD, NPD, FID and MS).
- Gas Chromatography sample preparation and introduction systems (Static and
dynamic headspace and SPME)
LC systems to cover many types of samples
- HPLC with Diode array Detector
- Preparative LC System for sample purification and fractionation
- IC with conductivity detector for charged species
Equipment and Facilities
Equipment and Facilities
AAS equipped to cover all types of samples
- Flame
- Graphite
- Hydride
- Solid sampling
Equipment and Facilities
Equipment and Facilities
Calibration
Reference Materials
Testing
Training
28
Services Provided by RM
Laboratory