INTRODUCTION TO FOOD ANALYSIS 1126

Steven C Seideman Extension Food Processing Specialist Cooperative Extension Service University of Arkansas
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FOOD COMPONENTS
Food consists primarily of water( moisture), fat (or oil), carbohydrate, protein and ash (minerals). Since food consists of these 5 components, it is important that we understand how these components are measured.

COMPOSITION OF FOODS
COMPONENT
Milk Beef Chicken Fish Cheese Cereal grains Potatoes Carrots Lettuce Apple Melon

% Water
87.3 60.0 66.0 81.8 37.0 10-14 78.0 88.6 94.8 84.0 92.8

%Carbohydrates %Protein % Fat % Min/Vit

5.0 0 0 0 2.0 58-72 18.9 9.1 2.8 15.0 6.0 3.5 17..5 20.2 16.4 25.0 8-13 2.0 1.1 1.3 0.3 0.6 3.5 22.0 12.6 0.5 31.0 2-5 0.1 0.2 0.2 0.4 0.2 0.7 0.9 1.0 1..3 5.0 0.5-3.0 1.0 1.0 0.9 0.3 0.4

MOISTURE DETERMINATION

Moisture Determination
Moisture or water is by far the most common component in foods ranging in content from 4 95%.

Moisture Content
The total moisture content of foods is generally determined by some form of drying method whereby all the moisture is removed by heat and moisture is determined as the weight lost.
% water =
wet weight of sample-dry weight of sample wet weight of sample
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Methods of Moisture Loss Measurement

Convection or forced draft ovens (AOAC) - Very simple; Most common Vacuum Oven -Sample is placed in oven under reduced pressure thereby reducing the boiling point of water. Microwave Oven -Uses microwave as a heat source; Very fast method Infrared Drying -Uses infrared lamp as a heat source; Very fast

PROTEIN ANALYSIS

PROTEINS
Proteins are made up of amino acids. Amino acids are the building blocks of protein. Nitrogen the most distinguishing element versus other food components (carbohydrates, fats etc) Nitrogen ranges in proteins : 13.4 - 19.1% Non-protein nitrogen: free amino acids, nucleic acids, amino sugars, some vitamins, etc. Total organic nitrogen = protein + non-protein nitrogen
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Types of Protein Analysis

Kjeldahl measures the amount of nitrogen in a sample. Lowry- measures the tyrosine/tryptophan residues of proteins.

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 Crude protein content Johan Kjeldahl (1883) developed the basic process Principle: total organic N released from sample and absorbed by acid

Total organic nitrogen - Kjeldahl method

Digestion: sulfuric acid + catalyst Neutralization and distillation; Sodium hydroxide Titration; Hydrochloric acid
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Total organic nitrogen - Kjeldahl method

Digestion
Sulfuric acid

Protein Heat, catalyst

(NH4)2SO4
(ammonium sulfate)

Protein N NH4+ + H2SO4 (NH4)2SO4

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Total organic nitrogen - Kjeldahl method

Neutralization and distillation
(NH4)2SO4 + 2NaOH 2NH3 + Na2SO4 + 2H2O
NH3 + H3BO3 NH4+ : H2BO3 + H3BO3
-

(boric acid)

(ammonium-borate complex) excess

Color change
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Total organic nitrogen - Kjeldahl method

Titration (direct titration) H2BO3 + H+ H3BO3
(HCl)

Calculation
moles HCl = moles NH3 = moles N in the sample
blank) 14g N %N = N*(HCl) (mL acid sample-mL acid 1000 g sample %N = N*(HCl) (mL acid sample-mL acid blank)
N*=Normality of HCl

mole

100

g sample

1.4
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Total organic nitrogen - Kjeldahl method Calculation

%Protein = %N conversion factor Conversion factor: generally 6.25
most protein: 16% N Conversion factor 6.25 6.38 5.33 5.52 5.17

egg or meat milk wheat soybean rice

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Kjeldahl Apparatus

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 Advantages:

Total organic nitrogen - Kjeldahl method

applicable to any foods simple, inexpensive accurate, official method for crude protein content

Disadvantages:
measuring total N not just protein N time consuming corrosive reagents
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Lowry Method
Principle: Color formation between tyrosine and tryptophan residues in protein and Biuret reagent and Folin-Ciocalteau phenol reagent (750 nm or 500 nm). Procedure
protein solution + biuret reagent
(20-100 g) room temp10 min

+ Folin reagent
50C 10 min

650 nm
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Lowry Method
Advantages
most sensitive (20-200g) more specific, relatively rapid

Disadvantages
color development not proportional to protein concentration color varying with different proteins interference (sugars, lipids, phosphate buffers, etc)

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Infrared Spectroscopy
Principle: absorption of radiation of peptide bond at mid-infrared (MIR) and near-infrared (NIR) bands Advantages
NIR applicable to a wide range of foods rapid, nondestructive little sample preparation

Disadvantages
expensive instruments calibration for different samples
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Crude Fat Analysis

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Fats
Fats refers to lipids, fats and oils. The most distinguishing feature of fats versus other components ( carbohydrates, protein etc) is their solubilty. Fats are soluble in organic solvents but insoluble in water.

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Solvent Extraction Methods

Sample preparation: Best under nitrogen & low temperature
Particle size reduction increases extraction efficiency Predrying sample to remove water is common.

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Solvent Extraction Methods

Solvent selection
Ideal solvent
high solvent power for lipids low solvent for other components easy to evaporate low boiling point nonflammable nontoxic good penetration into sample single component inexpensive non-hygroscopic

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Solvent Extraction Methods

Common Solvents
Ethyl ether - best solvent for fat extraction, more expensive, explosion, fire hazard, hygroscopic Petroleum ether - cheaper, more hydrophobic, less hygroscopic Hexane - soybean oil extraction

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Types of Fat Analysis

Extraction Methods Continuous Goldfinch Semi-Continuous- Soxhlet Discontinuous- Mojonnier Instrumental Methods Dielectric Infrared Ultrasound
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Solvent Extraction Methods

Continuous extraction: Goldfish method
Principle: Solvent continuously flowing over the sample with no build-up Advantages: fast, efficient. Disadvantages: channeling not complete extraction.

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Solvent Extraction Methods

Semicontinuous extraction: Soxhlet method
Principle: Solvent building up in extraction chamber for 5-10 min before siphoning back to boiling flask. Advantages: no channeling Disadvantages: time consuming
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Solvent Extraction Methods

Discontinuous extraction: Mojonnier method (wet method extraction)
Principle: a mixture of ethyl ether and petroleum ether in a Mojonnier flask Advantages: no prior removal of moisture Disadvantages: constant attention

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Instrumental Methods
Dielectric method
Principle: low electric current from fat

Infrared method
Principle: Fat absorbs infrared energy at a wavelength of 5.73 m

Ultrasound method
Principle: sound velocity increases with increasing fat content
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CARBOHYDRATE ANALYSIS

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Introduction
Next to water, carbohydrates are the most abundant food component
%carbohydrate=100% - (H2O + ash + fat + protein)

Types of carbohydrates include;

monosaccharide: glucose, fructose, galactose disaccharide: sucrose, lactose, maltose oligosaccharids: raffinose polysaccharide: starch, cellulose
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Ash and Mineral Analysis

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Definitions
Ash: total mineral content; inorganic residue
remaining after ignition or complete oxidation of organic matter

Minerals:
Macro minerals (>100 mg/day)
Ca, P, Na ,K, Mg, Cl, S

Trace minerals (mg/day)

Fe, I, Zn, Cu, Cr, Mn, Mo, F, Se, Si

Ultra trace minerals

Va, Tn, Ni, Sn, B

Toxic mineral
lead, mercury, cadmium, aluminum
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Ash Contents in Foods

Wheat flour, whole grain Macaroni, dry, enriched Milk, whole, fluid Butter, with salt Apple, raw with skin Banana, raw Egg, whole, raw Hamburger, regular, plain 1.6% 0.7% 0.7% 2.1% 0.3% 0.8% 0.9% 1.7%
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Methods for Determining Ash

Dry ashing
high temperature

Wet ashing
oxidizing agent and/or acid

Low-temperature plasma ashing

dry ashing in partial vacuum at low temperature

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Dry Ashing
Principles
High temperature (>525C) overnight (12-18 hr) total mineral content

Instrumentation
Muffle furnace Crucible
quartz porcelain steel nickel platinum
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General Procedure for Dry Ashing

1. 5-10g pretreated sample into a crucible 2. Ignite crucible to constant weight at ~550C for 12-18 hr 3. Cool in desiccator 4. Weigh cooled crucible
wt after ashing - crucible wt

% ash (db) =

Sample wt solid%/100

100
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Dry Ashing
Advantages
safe and easy no chemical many samples handled at one time resultant ash for further mineral analysis

Disadvantages
loss of volatiles interaction long time and expensive equipment
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COLOR
Color can be described in terms of hue, value and chroma; Hue is the aspect of color which we describe by words like green, blue, yellow and red Value or lightness describes the relationship between reflected and absorbed light, without regard to specific wavelength. Chroma describes reflection at a given wavelength and shows how much a color differs from gray.

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HUNTER L,a,b
The Hunter L,a,b system describes the color of a food in terms of L (100=white; 0= black), a (green- red) and b (blue to yellow).

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COLOR
More subjective color determination systems include; - Paint color match pages -The Pantone Matching System. - Actual photos of finished food products

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Sensory Properties
Trained Sensory Panels a few well trained people that characterize flavor, texture and odor versus like/dislike, Consumer Panels- usually consist of 200 plus people who determine like/dislike, desirability etc. Additional detailed information on sensory panels can be found in the module Sensory Evaluation of Foods; 1213
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SUMMARY
This module has presented the topic of Food Analysis by discussing why we analyze food, sampling and preparation, the components of food generally analyzed for (water, protein, fat, carbohydrates) and some general methods of analyzing the physical properties of food (color, viscosity and texture).
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