12 Juillet 2012, Brest

Chemical and physical

analysis for
food products

Philippe Mongondry
p.mongondry@groupe-esa.com 1
Techniques for food products: what for?

Quality control

Quantification of nutriments, vitamins

of compounds
Identification of contamination
Determination of ingredients

Authentication of origin of the product

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Foodstuffs should not contain micro-organisms or their
toxins or metabolites in quantities that present an
unacceptable risk for human health.
(EC Rule No 2073/2005)

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Many analytical chemical and physical techniques:

Electro-analysis Qty of ions Gravimetry Fat or water content

Electrophoresis separation Atomic spectrometry trace element
Molecular spectrometry emission (Fluo); diffusion (Raman) absorption (UV, IR RMN)
Mass Spectrometry Radiometry (14C) origin & date
X ray diffusion structural ID Rheometry Flow & structure
Sensory analysis Chromatography

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Preparation of sample for analysis is critical !!

Homogeneisation

Solubilisation

Separation

Analysis

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Physical and chemical analysis
• Chromatography
• Spectroscopy and related
microscopies (UV – visible – IR)
• SNIF NMR and Mass spectrometry

Sensory analysis
• Concepts and Basis

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Chromatography or HPLC

Extraction and preparation

in liquid media

Separation & Identification 7

Chromatography or HPLC
High Performance Liquid Chromatography

Different Types
• Partition chromatography
• Normal-phase chromatography
• Reversed-phase chromatography (RPC)
• Size-exclusion chromatography (SEC)
• Ion-exchange chromatography
• Bio-affinity chromatography

SEC

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 Chromatogram of Identification of
pesticide in cow milk polyphenols in wine by
UV detectors with HPLC

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Matter
Spectroscopy
and interactions

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 interactions light/matter
fluorescence
diffusion

photoemission

photon
transmission

absorption

c
E( J ) h. ( Hz ) h hc (m 1 )
diffraction
(m)
h : constante Planck; h= 6,62 x10-34 J.s-1
From atom to complex molecules

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 Biological Molecules
• Thousands of different molecules per cell, fast Renew
•Complex system
Biological specificity with 'allowed' movement and
conformation
• E(link etc...)reactions, biological and thermodynamic
parameters
• Particularity :
transformation of light energy (chlorophyll)
Proteins

Glucide
Lipids

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Nucleic acid
Spectroscopic principles
electromagnetic radiance Phenomena Frequency (Hz) Wave length
domain
Nuclear Magnetic Resonance
Radiofrequency 106 to 108 300 to 3 m
Nuclear Quadrupole Resonance
Electronic paramagnetic Resonance
Micro-ondes 1010 to 1012 300 to 0.3 mm
molecular rotations spectrum
Infrared molecular vibrations 1012 to 3 1014 300 to 0,8 m
Visible and ultraviolet Electronic Transitions (external e-) 3 1014 to 1016 800 to 10 nm
X Rays Electronic Transitions (core e-) 3 1016 to 1019 10 to 0.03 nm
0.03 to 0.003
Rays nuclear Transitions 1019 to 1022
nm

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From Far infrared to X-rays…
 Spectroscopic principles
Emission of large spectrum of photons (energy)

Transmission and reflection = nothing

Absorption of energy

UV absorption spectrum

Powerful photons No! but right ones Yes!

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 Spectroscopic principles

Construction of absorption spectrum

Polychromatic radiation
I I Abs

Large spectre of the Spectrale composition

source of transmise light

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Spectroscopy UV-visible HO

O
Absorption of UV by unsaturated bonds YES YES
O
NH2

NO YES O

Quantitative method,
Kinetic of reaction…

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 Infrared Spectroscopy
Principe:
Molecule under infrared radiation: vibration and rotation
Symmetrical Rocking Wagging
stretching

Antisymmetrical Scissoring Twisting

stretching

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http://fr.wikipedia.org/wiki/Spectroscopie_infrarouge
interactions light/matter
Atomic/molecules linkage movements due to which wave lengths in IR?

~3.3 m

3756 cm-1 3652 cm-1 1595 cm-1

~10 m ~30 m
~6 m
Fourier Transform InfraRed Spectroscopy
Fingerprint of molecules

spectrometer FTIR

Used for samples :

Gaz, liquid or solid in powder

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Quanti fy nutritional compounds by FTIR : polyphenols in apple

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 Quanti fy the quality of fruits by fast method : NIR

FTIR spectrum related to

°Brix, pH, dried matter
or starch content,
maturity, defaults…
Sucres
1.5
Sucres
R1
OH
1932
1 B R2

+
R
HO A 1455

0.5 es
an e 
OH

y
oc ll
nth p hy
A o
lor
0 Ch
553 1200
1270 Am2P3
675
-0.5 Am1P3
450 At0P3
976 At1P3
-1 At2P3
775
At3P3
At4P3
-1.5 At5P3
At6P3
S. Bureau, INRA Avignon
500 1000 1500 2000 2500 23
Longueurs d’onde (nm)
Quanti fy the quality of fruits by fast method : Ex. in apple

Total acid

Refractometric
index

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 IR microscopy = spatial
chemical distribution

50 m

1.1

1.0 Proteins
0.9
DNA
0.8
Lipids
0.7
Log(1/R)
0.6 DNA
50.5 m
0.4

0.3

0.2

0.1
Lipids
Proteins 3500 3000 2500 2000 1500 1000

Sections congelées (6µm) de muqueuse intestinale humaine Wavenumbers (cm-1)

M-P. Bralet and F. Le Naour, INSERM U775
Hôpital Européen Georges Pompidou, Paris;
Quanti fy the quality of milk by fast method : FTIR

•Le Milkoscan FT 120 de Foss : Fat, proteins, extrait sec content,

proteins
•Based on more than 15 years database to calibrate the apparatus

Much faster than standard chemical analysis of reference

Biocristallography with X-rays
Diffracted rays
3) recording X-rays
image
Cristal of protein

goniometer

Rayons X 2) diffraction
1) cristal

3D Structure of enzyme
RNA Polymerase II

4) Rebuilding 3D structure
Few examples of microscopies
Study of resistant bacteria by UV
In situ study of diffusion of antibiotic,
through bactéria membrane (first step
resistance to antibiotics).

Study of fermentation and cooking

of bread (bubbles of CO2) by X-
rays microtomography
SNIF NMR Site-Specific Natural Isotope Fractionation Nuclear Magnetic Resonance
Based on the absorption of deuterium in plants (Glucose or ethanol)
Irregular distribution of De on the Earth due to rotation

Addition of different type of sugar in Tequilas

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Mass Spectrometry
Main steps of the measurement Aims
Determination of the molecular
weight of big molecules (proteins)

Quick Identification based on

databases
Unknown sample

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Mass Spectrometry
Identification Coupling HPLC-MS
Reconstruction by affinity of pieces
Depend on position of the picks and ratio m/Z

Coupling techniques is powerful !!

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 Sensory analysis
What consumer understand from different information we give him ?

How his sensory experiments is influenced by the information he has ?

What is the impact of a new process or technology on his fondness ?

What is important in his purchase behavior ?

How to measure the sensory performance of products ?

How improve his loyalty ?

What consumer looks for ?

What does he discern in products ?

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 Sensory analysis
How objectively measure the tasting and the
sensorial characteristics of food products?

Factors which influence the choice of a food product ( Gains, 1994)

Consumer Context product

Habits Time of the day Sensorial characteristics

Culture place Nutriments
Personality With who Packaging
Current mood how
Physiology (allergy) Why what
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 Sensory analysis of Food products
Definition:
Evaluation of organoleptic properties of a food product by human senses
based on experimental design and statistical analysis (combination of
inferences or deductive reasoning and insight or specific cause and effect)

ICS 67.240 Sensory analysis

(ISO standard)
Glossary

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 Sensory analysis
How objectively measure the tasting and the sensorial characteristics of food products?

3 categories: Effective, affective and perception analysis

differences preferences Evocations Motivations

Descriptive Hedonic Qualitative
Test Test Test

Trained panel Naive consumers

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 Sensory analysis
Study consumer behavior and motivation

to get a better understanding of his reactions

Aims: Identify all reactions, all opinions that consumer have
Example : Reaction in front of the product
• Label, design
• Information
• Price
• Association of these different attributes
Which cap do you prefer ??

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Thank you for your attention

p.mongondry@groupe-esa.com

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