total fat quantitation using a new microwave assisted extraction workflow fast fat project · 2019....
TRANSCRIPT
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Total FAT Quantitation using a newMicrowave Assisted Extraction
Workflow
FAST FAT PROJECT
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•History of more than 100 yearsin Analytical Chemistry
www.thermounicam.pt
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. The Lab : Time is money
61%27%
6% 6%
SamplePreparation
Data Processing
Analysis
SamplingFrom: Ronald Majors “Overview on sample prep.” LG_GC. VOL. 9 . 1991
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The Modern Lab
• HPLC – HPLCMS – ICP- GCMS
• Modern technologies in ANALYSIS
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Lavoisier : law of conservation of mass
• Ovens, Heating baths, …
1789
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• Ovens, Heating baths, …
150 years ago Mendeleev
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German agricultural chemist Franz Ritter von
Soxhlet first introduced its Soxhlet laboratory
extractor in 1879 which deals in the
determination of milk fat.
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Standard Methods for Total Fat
Other fast-methodbutyrometric test,
or volumetric determination
• for milk: „Gerber“
• for cheese „Gulik“
• for cream: „Roeder“
• for skim milk: „Konrad“
• NIR/NMR
depending on user performance,
not very precise
Arbitration method
gravimetric test
• „Weibull-Stoldt“ (universal method)
• „Schmidt-Bondzynski“ (cheese)
• „Röse-Gottlieb“ (milk, cream)
• normal cheese must be analysed accord. to „Schmidt-Bondzynski“
• cheese with herbs/pepper must beanalysed accord. to „Weibull-Stoldt“
• AOAC Methods – NP similar to W-S and are the common reference
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Weibull-Stoldt Method Workflow
Weigh Sample
Hydrolysis Step
Filtration
Acid Wash
Dry (Oven)
SoxhletExtraction
Solvent Evaporation
Dry (Oven)
Weigh Residue
Data Process
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=O
HH
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Can we use MW M. A.E for TOTAL FAT Extraction ?
• The solvent of extraction is super-heated by microwave (aboveboiling point )
• Extractions Kinetics
k = Ae−
EaRT
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Microwaves and Heating
• The material can be :
• Reflective (metals)
• Absorbent (Water)
• Transparent (Hexane)
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Microwaves in the Lab
• CLOSED VESSEL Sample Digestion
• CLOSED VESSEL Sample Hydrolisis
• CLOSED VESSEL Extraction with Organicsolvents and stirring
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BOILING TEMPERATURE OF WATERvs. PRESSURE VAPOUR
Boiling temperature (°C)
Pressu
re (
bar)
0
10
20
30
40
50
60
70
80
90
0 50 100 150 200 250 300
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• Hypothesis: A fast and precise method for food and feed samples
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Proposed MAE Method Workflow
Weigh Sample
Dry (Oven) Solvent Evaporation
Hydrolysis Step Soxhlet Extraction
Weigh Residue
Data Process
Filtration
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Advantages
ETHOS X
Traditional
Hardware 12 Samples
3 Hs
16 hs – 2 Days
M.A.E
Traditional
Solvent
Solvent expense
M.A.E
Traditional
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Professional MW Balance 12 Position Evaporation
* Vacuum pump with pressure condensation for improved solvent recovery
Proposed Hardware for Total Fat
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Figures of Merit
Conclusion:
M.A.E proved to be easier, simpler and
equivalent to Soxhlet Methods for Cheese
samples
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Already tested and future
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Acknowledgements
U.B.I – Prof. J. Rodilla
AEMITEQ
Camillo Pirola – Diego Carnaroglio : Milestone