Department of Analytical Chemistry

Prof. Sena CAGLAR-ANDAC Assoc.Prof.Pelin KOSEOGLU YILMAZ

[email protected] [email protected]

Course References:

1- Food Analysis Fifth Edition Edited by S. Suzanne Nielsen, Springer 2017

2- Chemical Analysis of Food: Techniques and Applications, Edited by Yolanda Pico, second edition, Elsevier, 2020.

3- Handbook of FOOD ANALYSIS INSTRUMENTS Edited by Semih Ötles¸CRC Press, 2009

4- Related up-to-date publications

Introduction to Food Analysis,
Turkish and International Regulations,
Standards Related to Food Analysis,
Nutrition Labeling,
Evaluation of Analytical Data,
Sampling and Sample Preparation
1. INTRODUCTION
Reasons for analyzing foods

All food products require analysis of various characteristics (i.e., chemical composition,
microbial content, physical properties, sensory properties) as part of a quality
management program, from raw ingredients, through processing, to the final product.
 ANALYTICAL METHODS
 Making an appropriate choice of analytical technique for a specific application requires a

good knowledge of the various techniques

The success of any analytical method

relies on
 the proper selection and preparation
of the food sample,
 carefully performing the analysis,
 doing the appropriate calculations
 interpretation of the data

Fig.1.1. Method selection in food analysis

 Official methods are critical in the analysis of foods, to ensure that they meet the legal
requirements established by governmental agencies. Government regulations and international
standards most relevant to the analysis of foods are mentioned here
 CONSUMER DEMANDS
SAFE NUTRISIOUS HIGH QUALITY  OFFER A GOOD VALUE

 Consumer demand has driven significant growth in products making claims, many of which bring an increased
need for food analysis.

 For example, the consumer-driven, gluten-free claim has led to increased raw material/ingredient testing and

finished product testing, required to comply in the United States with the definition of this claim established by the
Food and Drug Administration.

 Many consumers are interested in the relationship between diet and health, including functional foods that may
provide health benefits beyond basic nutrition. The use of social media by consumers has changed expectations
and raised questions about the food supply. Such trends and demands by consumers increase the need for food
analysis and present some unique challenges regarding analytical techniques
For food companies to market safe, high-quality foods effectively in a national and
global marketplace, they must pay increasing attention to government regulations and
guidelines, and to the policies and standards of international organizations.

Food scientists must be aware of these regulations, guidelines, and policies related to

food safety and quality, and must know their implications for food analysis.

Government regulations related to the composition of foods include

 nutrition labeling,
 product claims,
 standards,
 inspection and grading,
 authenticity.
 In some cases, the cost of goods is
linked directly to the composition
as determined by analytical tests.
 in the dairy field, butterfat
content of bulk tank raw milk
determines how much money
the milk producer is paid for
Fig.1.2. Method selection in food analysis the milk.
 For flour, the protein content
can determine the price and
Analytical methods must be applied across the entire food food application for the flour.

supply chain to achieve the desired final product quality (Fig. These examples point to the
1.2). the food processor must understand the entire supply chain to importance for accurate
results from analytical
successfully manage product quality. testing.
 one must know the operating principles and
capabilities of the analytical methods
 to design experiments in product and process development,
 to assess results upon completion
 to evaluate the analytical data collected
 to determine whether product reformulation is needed or what parts of
 the process need to be modified for future tests.
TYPES OF SAMPLES ANALYZED IN A QUALITY
ASSURANCE PROGRAM FOR FOOD PRODUCTS
 SUPPLIER’S RESPONSIBILITIES
 Such specifications for raw materials/
ingredients come in various forms
 Downsizing in response to increasing within the food industry, with three
competition in the food industry often has commonly used forms described
pushed the responsibility for ingredient
quality to the suppliers.
 Companies increasingly rely on others to
supply high-quality and safe raw
ingredients and packaging materials.
 Many companies have select suppliers, on
whom they rely to perform the analytical
tests to ensure compliance with detailed
specifications for ingredients/raw materials.
 The ingredient semolina, which is
coarse-ground flour from durum
wheat (high protein), is used
especially to make pasta, but also for
other cereal grain-based products.
For this table, specific numbers are
not given, as they would be in the
actual documents for an ingredient.
 Ingredient specifications and COAs
are important for making specific
food products.
 For example, with the wrong starch
(i.e., with wrong specifications), a
specific food product may not
process correctly nor have the
desired finished product quality
attributes.
 Also, for example, if the COA
indicates the granulation size of a
specific lot of rolled oats is “out of
spec,” the finished granola bars may
not have the desired properties,
which can result in increased
PROPERTIES ANALYZED

product quality commonly involves testing the following: chemical composition/characteristics, physical properties, sensory
properties, and microbial quality.
 Objective of the
Assay

Characteristics of Standard
the Method Reference
Materials
Selection of the
method Validity of the
Select and Method
Prepare Sample ISO Certification
Sampling and
Sample Consideration of
preparation Food
Composition

Perform the
Official methods
STEPS IN THE Assay
ANALYSIS Chromatography

Spectroscopy and
spectrometry
Measures Of Standard Methods for the Examination of
Central Tendency Dairy Products , Standard Methods for the
Examination of Water and Wastewater
published by the American Public Health
Calculate and Association , Food Chemicals Codex ,
Interpret the Relıabılıty Of
Analysıs published by USP, Endorsed methods for
Results the chemical analyses of foods have been
compiled and published by The
Association of Official Analytical Chemists
Curve Fıttıng: (AOAC) International, and certain other
Regressıon nonprofit scientific organizations.
 TURKISH AND INTERNATIONAL
REGULATIONS
Turkish Regulations
 Laws and regulations reinforce the efforts of the food industry to provide wholesome foods, to inform
consumers about the nutritional composition of foods, and to eliminate economic frauds.

 CHAPTER ONE Food and Feed Safety, Responsibilities,Food Codex, Labeling and
Traceability, Presentation and Advertising, Protection of Consumer Rights
Regulations
CODEX ALIMENTARIUS COMMISSION (CAC)
 Established in 1963 jointly by the United Nations
Food and Agriculture Organization (FAO) and World
Health Organization (WHO).
 184 member countries and one member organization
(European Union).
 The commission is responsible for the standardization of food-
related practices in the World in terms of health and
technology. Prepared by the commission for this aim, "Codex
Alimentarius Standards" is a reference document for
all countries in the World concerning safe food production.

https://www.fao.org/fao-who-codexalimentarius/committees/committee/en/?committee=CAC
 Türkiye became a member of CAC on October 01st, 1963. Being a
contact point for CAC, General Directorate of Food and Control
represents Türkiye in CAC meetings.
 While creating the national legislation of Türkiye, Codex
Alimentarius norms and approaches are taken as a basis. In order
to take part in international approaches and to have a say in
international trade, participation of Türkiye in CAC and relevant sub-
committee activities carries great importance.
https://www.fao.org/faolex/res
ults/details/en/c/LEX-
FAOC193956/
https://www.fao.org/faolex/res
ults/details/en/c/LEX-
FAOC106144
https://www.fao.org/faolex/res
ults/details/en/c/LEX-
FAOC193956/
https://www.fao.org/faolex/res
ults/details/en/c/LEX-
FAOC106144
 INTERNATIONAL REGULATIONS
 European Food Safety Authority (EFSA); https://www.efsa.europa.eu/en

U.S. Food and Drug Administration (FDA); https://www.fda.gov/food

SPECIAL STANDARDS IN CODEX ALIMENTARIUS

 Special standards within Codex Alimentarius cover the following products:

• Cereals, legumes and similar products with vegetable proteins,
• Fat-oil and relevant products,
• Fish and fish products,
• Fresh fruits and vegetables,
• Processed and Frozen fruits and vegetables,
• Fruit juices,
• Meat and meat products; soups and broth,
• Milk and dairy products,
• Sweets, cocoa products, chocolate and other miscellaneous products.

Product standards are defined in a specific format in CAC Procedural
Guidebook. This format covers the information such as scope, definition, basic
composition, food additives, contaminants, hygiene, weight and measures,
labelling, sampling and analysing methods.
 NUTRITION LABELLING
 Nutrition labeling regulations differ in countries around the world.
 Codex provides guidance on the compositional requirements of foods so that
they are nutritionally safe. Codex also provides guidance on general
labelling of foods and the health or nutrient claims producers make on labels,
with terms such as "low fat", "high fat" etc.
 Codex guidance ensures that consumers understand what they are buying
and that "it is what it says it is".
 . The Codex Committee on Food Labelling (CCFL) sets standards and
guidelines for nutrition information on food packages enabling consumers to
make informed food choices.
 NUTRITION LABELLING
The regulations,as related to food analysis, focusing on the following:
 1. What nutrients must be analyzed
 2. How samples are to be collected
 3. What methods of analysis are to be used
 4. How data are to be reported
 5. How data can be used to calculate caloric content
 6. How data can be used for claims made on the food label

Nutrition
labelling

Daily values Nutrient

Rounding Caloric Protein Compliance
and serving Health Claims Content
Rules Content Quality
sizes Claims
SAMPLING AND SAMPLE PREPARATION
 The small portions taken for analysis are referred to as samples, and the
entire lot or the entire production for a certain period of time, in the case of
continuous processes, is called a population. The process of taking samples
from a population is called sampling.
 By sampling only a fraction of the population, a quality estimate can be
obtained accurately, quickly, and with less expense and personnel time than
if the total population were measured.
 The International Union of Pure and Applied Chemistry (IUPAC) defines a
sampling plan as: “A predetermined procedure for the selection, withdrawal,
preservation, transportation, and preparation of the portions to be removed
from a lot as samples”
  The two primary objectives of sampling are often to
estimate the average value of a characteristic and
determine if the average value meets the
specifications defined in the sampling plan.

Nature of Population and Product

The ideal population and product: homogenous

The most populations and products that are sampled are heterogeneous
PREPARATION OF SAMPLES
A. General Size Reduction Considerations
If the particle size or mass of the sample is too large for analysis, it must be reduced in bulk or
particle size to obtain a smaller quantity for analysis, the sample can be spread on a clean surface
and divided into quarters. The two opposite quarters are combined. If the mass is still too large for
analysis, the process is repeated until an appropriate amount is obtained. This method can be
modified for homogeneous liquids by pouring into four containers and can be automated
B. Grinding
 Applications for Grinding Equipment

Mills differ according to their mode of action, being classified as a burr, hammer, impeller,
cyclone, impact, centrifugal, or roller mill
 Determination of Particle Size

1. Particle size is controlled in certain mills by adjusting the distance between burrs or blades or by
screen mesh size/number. The mesh number is the number of square screen openings per linear
inch of mesh. The final particles of dried foods should be 20 mesh for moisture, total protein, or
mineral determinations. Particles of 40 mesh size are used for extraction assays such as lipid and
carbohydrate estimation.
PREPARATION OF SAMPLES

 Determination of Particle Size

2. To obtain more accurate size data for smaller particles (<50 μm), characteristics that correlate
to size are measured, and thus size is measured indirectly . Surface area and zeta potential
(electrical charge on a particle) are characteristics that are commonly used. Zeta potential is
measured by an electroacoustic method whereby particles are oscillated in a high frequency
electrical field and generate a sound wave whose amplitude is proportional to the zeta
potential.
C. Enzymatic Inactivation
 Food materials often contain enzymes that may degrade the food components being analyzed.
Enzyme activity therefore must be eliminated or controlled using methods that depend on the
nature of the food.
 Heat denaturation to inactivate enzymes and freezer storage (−20 to −30 C) for limiting
enzyme activity are common methods. However, some enzymes are more effectively
controlled by changing the pH or by salting out. Oxidative enzymes may be controlled by
adding reducing agents.
PREPARATION OF SAMPLES
D. Lipid Oxidation Protection
Lipids present particular problems in sample preparation. High-fat foods are
difficult to grind and may need to be ground while frozen.
Unsaturated lipids are sensitive to oxidative degradation and should be protected
by storing under nitrogen or vacuum.
Antioxidants may stabilize lipids and may be used if they do not interfere with the
analysis.
Light-initiated photooxidation of unsaturated lipids can be avoided by controlling
storage conditions. In practice, lipids are more stable when frozen in intact tissues
rather than as extracts. Therefore, ideally, unsaturated lipids should be extracted
just prior to analysis. Low-temperature storage is generally recommended to
protect most foods.
PREPARATION OF SAMPLES
 Microbial Growth and Contamination
 Microorganisms are present in almost all foods and can alter the
sample composition. Likewise, microorganisms are present on all
but sterilized surfaces, so sample cross-contamination can occur if
samples are not handled carefully.
 Freezing, drying, and chemical preservatives are effective controls
and often a combination of these is used.
 The preservation methods used are determined by the probability
of contamination, the storage conditions, storage time, and the
analysis to be performed
PREPARATION OF SAMPLES

Time spent
Sources of error

33
 the most common techniques for sample
preparation, including:
Dilution
Filtration/centrifugation (particulate removal)
Protein precipitation
Liquid/liquid extraction
Support-assisted liquid/liquid extraction (SALL)
Solid phase extraction
 Each of these techniques has value in its own right, and each may be the most suitable choice
for a particular application. There are many factors that can influence the choice of one
technique over the other, and only the user can weigh these factors to arrive at the optimum
decision. Some of the more common factors include:
Simplicity — how skilled must the user of the technique be?
Speed — how fast can samples be processed?
Selectivity — how clean an extract is required?
Sensitivity — how small a final extract volume is required?
Complexity of method development — what skill levels
exist in the lab?
Automatability — must the technique be run
unattended?