Physical and Chemical Methods

of Food Analysis
Assoc. Prof. Dr. PHAN TẠI HUÂN
Faculty of Chemical Engineering and Food Technology
Nong Lam University - HCMC

Course Objectives
• Provide principles relating to the separation and quantification
of various constituents within foods.
• General understanding of basic instrumental methods relating
to food analysis.
• Develop good laboratory skills and control of quantitative
techniques.
• Develop your knowledge of food analysis associated with the
procedures.

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 Course Introduction
Recommended texts
• Introduction to the Chemical Analysis of Foods. Suzanne
Nielsen, Jones and Bartlett Publishers, London, 1994.
(FST Library)
• Food Analysis. Suzanne Nielsen, Fourth Edition, Springer,
NY, 2010. (NLU Library)
• Food analysis: Theory and practice, Y. Pomeranz & C. E.,
Meloan An Aspen Publication, 2000. (Google book).
• Fundamentals of Analytical Chemistry, D.A. Skoog et al.,
Thomson – Brook/Cole, 2004.

Attendance requirements
• Class attendance: 2 units (30 hrs)

Course Introduction
Class-schedule
– See attachment
Assessment
• Method Weighting
– Quiz:
– Mid-term test:
– Lab report:
– Final examination:

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 Lecture 1:
Introduction to Food Analysis
• Reading : Chapter 1 and 2 in Book “Introduction to the
Chemical Analysis of Foods”, Suzanne Nielsen, Jones and
Bartlett Publishers, London, 1994.

Why Analyze Foods?

• Nutritional Analysis:
– nutritional information labeling and surveillance
• Vitamins & Minerals Analysis
• Pesticide Residue Analysis
• Monitoring Intentional and Non-intentional
Additives:
– Colorants, sweetners, preservatives etc.
– Veterinary Residues – antibiotics, drugs
– Toxins & Carcinogens
– Microbial, acrylamide

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 Why Analyze Foods?
• Nutrient Analysis
– Determine nutrient content to support health claims
• Quality Assurance
– Determine quality, composition and consistency of raw
materials
– Process Control Samples: Determine how processing
impacts the product
– Finished Products: Does the product meet the legal
requirements?
– Competitors Samples: New product development
– Complaint Samples: How does this sample differ from
samples with no problems?
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Food and the Law

Primary Agencies in Vietnam:
• Food Safety Agency - Ministry of Health Portal.
http://portal.vfa.gov.vn
• Plant Protection Department - Ministry of Agriculture
and Rural Development.
http://www.ppd.gov.vn/
• Directorate for Standards, Metrology and Quality –
Ministry of Science and Technology.
http://www.tcvn.gov.vn/

Example 8

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Food and the Law

Primary Agencies in US:

1. Food & Drug Administration (FDA)

– Food and Drug Act (FDA) 1906
– Federal Food, Drug and Cosmetic Act (FFD&C)
1938
Set Standards of Identity
– Nutrition Labeling Act 1990
www.fda.gov

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 Food and the Law
Primary Agencies Regulating Foods in US

2. United States Department of Agriculture (USDA)

– The Food Safety and Inspection Service (FSIS)
Meat, poultry and egg products
http://www.fsis.usda.gov

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Food and the Law

Primary Agencies Regulating Foods in US

3. Environmental Protection Agency (EPA)

– Federal Insecticide, Fungicide and Rodenticide Act
– Tolerances for pesticide residues
www.epa.gov

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 Food and the Law
International:
• The Codex Alimentarius (Latin: "food code")
The Codex Alimentarius Commission was created in
1963 by FAO and WHO to develop food standards,
guidelines and related texts such as codes of practice
under the Joint FAO/WHO Food Standards
Programme.
http://www.codexalimentarius.net

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Resource Materials Available for the Food Analyst

1. Books
– Introduction to the Chemical Analysis of Foods
– Food analysis: Theory and practice
2. Official Methods of Analysis
– AOAC Intl: Association of Official Analytical Chemists
International.
Authoritative source of analytical methods used worldwide
(contains over 2,700 collaboratively tested methods that
will perform with accuracy and precision (Example)
3. Research Journals (Example)
4. Trade Journals
5. Manufactures catalogs and web sites
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 Trends and Demands
Consumer driven
relationship between diet and health
– nutrient content used
– health claim information important
Examples:
low fat foods have been developed to satisfy consumer
requirement
– analytical methods determine and characterise fat content,
making health claims possible
– fat substitutes produce challenges for accurate fat content
measurement

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Trends and Demands

Food industry driven:
• management of quality from raw materials to final product
– quality control and quality assurance are only a part of a
detailed quality management system
• analytical methods must be applied
• select suppliers of food ingredients
– they perform the analytical tests
– ensure compliance with food company’s ingredient
Specifications

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 Stages in Food Analysis
Stages that may be required in the analysis of foods are:
1. Setting the protocol.
2. Sampling the food.
3. Preparing the sample in readiness for extraction of the chosen
analyte or compound of interest.
4. Extraction of the compound of interest .
5. Separation from, or removal of, substances interfering with the
detection of the compound of interest in the extract.
6. Detection (recognition or visualisation) of the compound of
interest.
7. Identification and/or quantification of the compound of interest.
8. Recording and processing the information.
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Defining the Stages in Food Analysis

Setting the Protocol:
• It is important to have a clearly defined protocol and to adhere
to it, so that the analysis can be reported unambiguously,
verified by the analyst, and, if necessary, reproduced for
verification by other analysts.

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 Criteria for Choice of Food Analysis Methods
Characteristic Critical Questions
Inherent properties
Specificity/ Is the property being measured the same as that claimed to
selectivity be measured, and is it the only property being measured?
Are there interferences?
What steps are being taken to ensure a high degree of
specificity?
Precision What is the precision of the method? Is there within-batch,
batch-to-batch, or day-to-day variation?
What step in the procedure contributes the greatest
variability?
Accuracy How does the new method compare in accuracy to the old or
a standard method?
What is the percent recovery?
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Criteria for Choice of Food Analysis Methods

Characteristic Critical Questions
Applicability of
method to laboratory
Sample size How much sample is needed?
Is it too large or too small to fit your needs?
Does it fit your equipment and/or glassware?
Can you obtain representative sample?
Reagents Can you properly prepare them?
What equipment is needed? Are they stable? For how long
and under what conditions?
Equipment Is the method very sensitive to slight or moderate changes
in the reagents?
Do you have the appropriate equipment?
Are personnel competent to operate equipment?
Cost What is the cost in terms of equipment, reagents, and28
personnel?

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 Criteria for Choice of Food Analysis Methods
Characteristic Critical Questions
Usefulness
Time required How fast is it? How fast does it need to be?
Reliability How reliable is it from the standpoints of precision and
stability?
Need Does it meet a need or better meet a need?

Personnel
Safety Is any change in method worth the trouble of the change?
Are special precautions necessary?
Procedures Who will prepare the written description of the procedures
and reagents?
Who will do any required calculations?

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Defining the Stages in Food Analysis

Sampling the Food:
• This is the process of preparing a representative portion of the
whole food for analysis.
• This sample is usually re-sampled by the analyst (the sample
for analysis) and may need treatment before the target
compounds can be extracted.

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 Defining the Stages in Food Analysis
Preparation of the Sample for Extraction:
• The definition of sample preparation is ambiguous in the
literature, often covering all processes up to and including the
separation stage.
• The definition of sample preparation for extraction here is “the
execution of procedures necessary to prepare the original
sample for extraction.”
– Such processes include grinding, digestion, and
centrifugation. Occasionally, mainly for liquid foods, no
preparation for extraction is required.

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Defining the Stages in Food Analysis

Extraction:
• An extraction process used in collecting together relevant
subjects was “one where a part of the sample is removed from
the whole starting sample.”
• It may be the part containing the compounds of interest or it
may be an unwanted part being discarded, leaving a less
complex and usually more concentrated remainder for further
study.
Direct Analysis without Extraction:
• The analyte can be in sufficient concentration, and free from
interference from the matrix, usually in a liquid food, that no
extraction stage is necessary.
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 Defining the Stages in Food Analysis
Separation:
• The term separation is reserved for chromatographic and
electrophoretic processes where the main objective is not to
remove or extract something for further stages of analysis, but
to finally resolve components of mixtures for detection and
identification.

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Defining the Stages in Food Analysis

Detection for Identification and/or Quantification:
• The signal recorded when a component of the sample is
registered (recognised, standardised or calibrated) above a
base line, and the signal content is converted into qualitative
or quantitative information.

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 Defining the Stages in Food Analysis
Direct Detection by Remote Sensing of the Food Sample.
• If the analyte can be recognised (detected) in the food sample
prepared for analysis by a sensing probe, then the required
analytical data can be extracted directly without the need for
physical, chemical, or biochemical intervention.
• This can be considered to be “virtual extraction or virtual
removal of interference.” Such methods have the potential to
be rapid, economical in time and resources, and ideal for
automation.

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Defining the Stages in Food Analysis

Recording and processing the information.
• Analytical results are incomplete without an estimate of their
reliability. The experimenter must provide some measure of
the uncertainties associated with computed results if the data
are to have any value.

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