Food analysis is the discipline dealing with the development, application ands t u dy of a nal yt i ca l pr ocedur es f or char act er i z ing

t he pr op er t i es of f oods a nd t heir constituents. These analytical procedures are used to provide information about a widevariety of different characteristics of foods, including their composition, structure,physicochemical properties and sensory attributes. This information is critical to our rational understanding of the factors that determine the properties of foods, as well asto our ability to economically produce foods that are consistently safe, nutritious anddesirable and for consumers to make informed choices about their diet. The objectiveof this course is to review the basic principles of the analytical procedures commonlyused to analyze foods and to discuss their application to specific food components, e.g. lipids, proteins, water, carbohydrates and minerals. The following questions will beaddressed in this introductory section: Who analyzes foods? Why do they analyzefoods? What types of properties are measured? How does one choose an appropriateanalytical technique for a particular food? 1.1. Reasons for Analyzing Foods Foods are analyzed by scientists working in all of the major sectors of the foodindustry including food manufacturers, ingredient suppliers, analytical servicelaboratories, government laboratories, and University research laboratories. Thevarious purposes that foods are analyzed are briefly discussed in this section. 1.1.1. Government Regulations and Recommendations Government regulations and recommendations are designed to maintain thegeneral quality of the food supply, to ensure the food industry provides consumerswith foods that are wholesome and safe, to inform consumers about the nutritionalcomposition of foods so that they can make knowledgeable choices about their diet, toenable fair competition amongst food companies, and to eliminate economic fraud.T her e ar e a nu mb er of G over n ment D ep ar t ments R es p ons i bl e f or r egu la t i ng t he composition and quality of foods, including the Food and Drug Administration (FDA),the United States Department of Agriculture (USDA), the National Marine Fisheries Service (NMFS) and the Environmental Protection Agency (EPA). Each of thesegov er nme nt a ge nci es is r es pons i bl e for r egu la t i ng pa r tic ular s ect or s of t he foodindustry and publishes documents that contain detailed information about ther egula t ions a nd r ec ommenda t i ons p er t ai ni ng t o t he foods pr oduce d wi t hi n t hos esectors. These documents can be purchased from the government or obtained on-linefrom the appropriate website. Standards Government agencies have specified a number of voluntary and mandatorystandards concerning the composition, quality, inspection, and labeling of specific foodproducts.

Mandatory Standards: - Standards of Identity. These regulations specify the type and amounts of ingredients that certain foods must contain if they are to be called by a particular nameon the food label. For some foods there is a maximum or minimum concentration of acertain component that they must contain, e.g., peanut butter must be less than 55%fat, ice-cream must be greater than 10% milk fat, cheddar cheese must be greater than 50% milk fat and less than 39% moisture.

- Standards of Quality. Standards of quality have been defined for certainfoods ( e.g., canned fruits and vegetables) to set minimum requirements on the color,tenderness, mass and freedom from defects.

- Standards of Fill-of-Container. T h e s e s t a n d a r d s s t a t e h o w f u l l a container must be to avoid consumer deception, as well as specifying how the degreeof fill is measured.

Voluntary Standards: - Standards of Grade. A number of foods, including meat, dairy productsand eggs, are graded according to their quality, e.g. from standard to excellent. For example meats can be graded as prime, choice, select, standard etc accordingto their origin, tenderness, juiciness, flavor and appearance. There are clear definitionsassociated with these descriptors that products must conform to before they can begiven the appropriate label. Specification of the grade of a food product on the label is voluntary, but many food manufacturers opt to do this because superior grade productscan be sold for a higher price. The government has laboratories that food producerssend their products too to be tested to receive the appropriate certification. This serviceis requested and paid for by the food producer.

Nutritional Labeling In 1990, the US government passed the Nutritional Labeling and EducationAct (NLEA), which revised the regulations pertaining to the nutritional labeling of f oods , a nd ma d e it ma n dat or y f or al mo st all f ood pr oduct s t o ha v e s ta nda r diz ed nutritional labels. One of the major reasons for introducing these regulations was sothat consumers could make informed choices about their diet. Nutritional labels statet he t ota l ca l or if i c va lu e of t he f ood, as wel l as t ot al fat , s at ur at ed fa t , c hol est er ol, sodium, carbohydrate, dietary fiber, sugars, protein, vitamins, calcium and iron. Thelabel may also contain information about nutrient

content claims (such as low fat,low sodium high fiber fat free etc), although government regulations stipulatet he mi ni mu m or max i mu m a mou nt s of s pec if i c f ood comp one nt s t ha t a f ood mu st contain if it is to be given one of these nutrient content descriptors. The label may alsoc o nt a i n cer ta i n F DA ap pr oved h ea lt h cla i ms ba s ed on li nks bet we en s pec i fi c f oodcomponents and certain diseases ( e.g., ca l ci u m a nd os t eop or os is , s odi u m a n d hi ghblood pressure, soluble fiber and heart disease, and cholesterol and heart disease). Theinformation provided on the label can be used by consumers to plan a nutritious andba la nce d di et , t o a voi d ov er co ns u mpt i on of f ood c omp onent s l i nked wit h h ea lt hproblems, and to encourage greater consumption of foods that are beneficial to health.

Authenticity The price of certain foods is dictated by the quality of the ingredients that theycontain. For example, a packet of premium coffee may claim that the coffee beans arefrom Columbia, or the label of an expensive wine may claim that it was produced in acertain region, using a certain t ype of grapes in a particular year. How do we verifythes e claims? There are many instances in the past where manufacturers have madefalse claims about the authenticity of their products in order to get a higher price. It ist h e r e f o r e i mp or tant t o ha ve a nal ytical t echni qu es t hat ca n b e used t o t est t h e authenticity of certain food components, to ensure that consumers are not the victimsof economic fraud and that competition among food manufacturers is fair. Food Inspection and Grading T he g over nment ha s a Food Inspection and Grading Service that routinelyanalyses the properties of food products to ensure that they meet the appropriate lawsa n d r egu la t i ons . H enc e, bot h gover n ment a genci es a nd fo od ma nufa ct ur er s ne edanalytical techniques to provide the appropriate information about food properties. Themost important criteria for this type of test are often the accuracy of the measurementsand the use of an official method. The government has recently carried out a survey of ma n y o f t he of fi ci a l a na l yt ic a l t ec h ni qu es dev el op e d t o a na l yz e f oods , a nd h a s s p ec ifi ed whi c h t ech ni qu es mu st be us ed t o a nal yz e cert ai n f oo d co mp on ent s for labeling purposes. Techniques have been chosen which provide accurate and reliableresults, but which are relatively simple and inexpensive to perform. 1.1.2. Food Safety One of t he mos t impor ta nt r eas ons f or analyzi ng f oo ds fr om b o t h t h e consumers and the manufacturers standpoint is to ensure that they are safe. It would beeconomically disastrous, as well as being rather unpleasant to consumers, if a foodmanufacturer sold a product that was harmful or toxic. A food may be considered to beunsafe because it contains harmful microorganisms (e.g.,Listeria, Salmonella), toxicchemicals ( e.g., pesticides, herbicides) or extraneous matter (e.g.,glass, wood, metal,insect matter).

It is therefore important that food manufacturers do everything they canto ensure that these harmful substances are not present, or that they are effectivelyel i minat ed b ef or e t he f oo d is c ons u med. T hi s ca n be a chie ved by f ol l owi ng good manufacturing practice regulations specified by the government for specific foodproducts and by having analytical techniques that are capable of detecting harmfulsubstances. In many situations it is important to use analytical techniques that have ahigh sensitivity, i.e., t ha t ca n r el ia b l y det ect l ow l e vel s of har mf ul ma t er ia l. F ood manufacturers and government laboratories routinely analyze food products to ensurethat they do not contain harmful substances and that the food production facility isoperating correctly 1.1.3. Quality control The food industry is highly competitive and food manufacturers areco nt i nua ll y t r yi ng t o i ncr eas e t heir ma r ket -s har e a nd pr of it s. T o do t hi s they must ensure that their products are of higher quality,less expensive, and more desirable thantheir competitors, whilst ensuring that they are safe and nutritious. T o me et t hes er i gor ou s s t a nda r ds f ood ma nu fa ct ur er s need a na l yt i ca l t ec hni ques t o a na l yz e foodmaterials before, during and after the manufacturing process to ensure that the finalpr odu ct meet s t he des ir ed s ta nda r ds. I n a f ood fact or y o ne s t ar t s wit h a nu mber of different raw materials, processes them in a certain manner (e.g. heat, cool, mix, dry), packages them for consumption and then stores them. The food is then transported to awarehouse or retailer where it is sold for consumption.One of the most important concerns of the food manufacturer is to produce afinal product that consistently has the same overall properties, i.e. appearance, texture,f la vor a nd s hel f li f e. Whe n we pur chas e a pa rt ic ular food pr odu ct we expect it s pr oper t i es t o be t he s a me ( or ver y s i mi l ar ) to pr evi ou s t i mes, a nd not t o va r y fr ompurchase-to-purchase. Ideally, a food manufacture wants to take the raw ingredients,process them in a certain way and produce a product with specific desirable properties.Unfortunately, the properties of the raw ingredients and the processing conditions varyfrom time to time which causes the properties of the final product to vary, often in anunpredictable way. How can food manufacturers control these variations? Firstly, theycan understand the role that different food ingredients and processing operations playin determining the final properties of foods, so that they can rationally control themanufacturing process to produce a final product with consistent properties. This typeof information can be established through research and development work (see later).Secondly, they can monitor the properties of foods during production to ensure thatthey are meeting the specified requirements, and if a problem is detected during theproduction process, appropriate actions can be taken to maintain final product quality. Characterization of raw materials. Manufacturers measure the properties of incoming raw materials to ensure that they meet certain minimum standards of qualitythat have previously been defined by the manufacturer. If these standards are not metthe manufacturer rejects the material. Even when a batch of raw materials has beenaccepted, variations in its properties might lead to changes in the properties of the finalproduct. By analyzing the raw materials it is often possible to predict their subsequent

behavior during processing so that the processing conditions can be altered to producea fi na l pr odu ct wit h t he des ir ed pr oper ti es. F or exa mp le, t he c ol or of p ot at o chips d e p e n d s o n t h e c o n c e n t r a t i o n o f r e d u c i n g s u g a r s i n t h e p o t a t o e s t h a t t h e y a r e manufactured from: the higher the concentration, the browner the potato chip. Thus itis necessary to have an analytical technique to measure the concentration of reducings u gar s i n t he pota t oes s o t hat t he fr yi ng co ndit i ons ca n be a lt er ed t o pr odu c e t he optimum colored potato chip. Monitoring of food properties during processing. It is advantageous for food manufacturers to be able to measure the properties of foods during processing.T hus , if a ny pr obl e m devel op s, t hen it ca n be qui c kl y det ect ed, a nd t he pr ocess adjusted to compensate for it. This helps to improve the overall quality of a food and toreduce the amount of material and time wasted. For example, if a manufacturer wereproducing a salad dressing product, and the oil content became too high or too lowt h e y w o u l d w a n t t o a d j u s t t h e p r o c e s s i n g c o n d i t i o n s t o e l i m i n a t e t h i s p r o b l e m. Traditionally, samples are removed from the process and tested in a quality assurancelaboratory. This procedure is often fairly time-consuming and means that some of thepr odu ct is us ua ll y was t ed b ef or e a pa rt i cu lar pr oble m bec omes a ppa r e nt . F or t hisreason, there is an increasing tendency in the food industry to use analytical techniqueswhich are capable of rapidly measuring the properties of foods on-line, without havingt o r e m o v e a s a m p l e f r o m t h e p r o c e s s . T h e s e t e c h n i q u e s a l l o w p r o b l e m s t o b e determined much more quickly and therefore lead to improved product quality and lesswas t e. T he i dea l cr it er ia f or a n on- li ne t ec hni qu e is t hat it b e ca pa ble of ra pi d a n dpr ec is e mea s ur eme nt s, it is non-i nt r us i ve, it is nondes t ru ct i ve a nd t ha t it ca n beautomated. Characterization of final product. O nc e t he pr odu ct has bee n ma de it is important to analyze its properties to ensure that it meets the appropriate legal andlabeling requirements, that it is safe, and that it is of high quality. It is also important toensure that it retains its desirable properties up to the time when it is consumed. A system known as Hazard Analysis and Critical Control Point (HACCP)h a s b e e n d e v e l o p e d , w h o s e a i m i s t o s y s t e m a t i c a l l y i d e n t i f y t h e i n g r e d i e n t s o r processes that may cause problems (hazard analysis), assign locations (critical controlpoints) within the manufacturing process where the properties of the food must be m e a s u r e d t o e n s u r e t h a t s a f e t y a n d q u a l i t y a r e ma i n t a i n e d , a n d t o s p e c i f y t h e appropriate action to take if a problem is identified. The type of analytical technique required to carry out the analysis is often specified. In addition, the manufacturer must keep detailed documentation of the performance and results of these tests. HACCP was initially developed for safety testing of foods, but it or similar systems are alsonow being used to test food quality. 1.1.4. Research and Development I n r ece nt yea r s, t her e ha ve bee n si gni fi ca nt cha nges i n t he pr ef er enc es of consumers for foods that are healthier, higher quality, lower cost and more exotic.I ndi vi du a l food ma nufa ct ur er s mus t r es pond ra pi dl y t o t hes e c ha n ges

i n or der t oremain competitive within the food industry. To meet these demands foodmanufacturers often employ a number of scientists whose primary objective is to carryout research that will lead to the development of new products, the improvement of existing products and the reduction of manufacturing costs.Many scientists working in universities, government research laboratories andlarge food companies carry out basic research. Experiments are designed to provideinformation that leads to a better understanding of the role that different ingredientsand processing operations play in determining the overall properties of foods. Researchis mainly directed towards investigating the structure and interaction of foodingredients, and how they are effected by changes in environment, such astemperature, pressure and mechanical agitation. Basic research tends to be carried outon simple model systems with well-defined compositions and properties, rather thanreal foods with complex compositions and structures, so that the researchers can focuso n p a r t i c u l a r a s p e c t s o f t h e s y s t e m. S c i e n t i s t s w o r k i n g f o r f o o d c o m p a n i e s o r ingredient suppliers usually carry out product development. Food Scientists working inthis area use their knowledge of food ingredients and processing operations to improvethe properties of existing products or to develop new products. In practice, there is agreat deal of overlap between basic research and product development, with the basicr es ear ch er s pr ovidi ng i nf or mat i on t hat ca n be us e d by t he pr oduct devel op er s torationally optimize food composition and properties. In both fundamental research andpr oduct dev el op ment a nal yt ica l t ec hni ques a r e nee ded t o c ha ra ct er i ze t h e over a l l properties of foods (e.g., color, texture, flavor, shelf-life etc.), to ascertain the role that each ingredient plays in determining the overall properties of foods, and to determinehow t he pr op er t i es of f oods a r e aff ect e d by var i ous pr oces s i ng con dit ions ( e.g.,storage, heating, mixing, freezing). 1.2 Properties Analyzed F ood a na lyst s ar e i nt er est ed in obt a i ni ng infor mat i on a bout a var i et y of different characteristics of foods, including their composition, structure,physicochemical properties and sensory attributes. 1.2.1 Composition The composition of a food largely determines its safety, nutrition,physicochemical properties, quality attributes and sensory characteristics. Most foodsare compositionally complex materials made up of a wide variety of different chemicalc o n s t i t u e n t s . T h e i r c o m p o s i t i o n c a n b e s p e c i f i e d i n a n u m b e r o f d i f f e r e n t w a y s depending on the property that is of interest to the analyst and the type of analyticalprocedure used: specific atoms (e.g.,Carbon, Hydrogen, Oxygen, Nitrogen, Sulfur,S odiu m, et c. ); s pec ifi c mol ec ul es ( e.g.,water, sucrose, tristearin, lactoglobulin),types of molecules (e.g.,fats, proteins, carbohydrates, fiber,minerals), or specific substances (e.g., peas, flour, milk, peanuts, butter). Governmentregulations state that the concentration of certain food components must be stipulatedon the nutritional label of most food products, and are usually reported as specificmolecules (e.g.,vitamin A) or types of molecules (e.g.,proteins).

1.2.2 Structure The structural organization of the components within a food also plays a largerole in determining the physicochemical properties, quality attributes and sensorycharacteristics of many foods. Hence, two foods that have the same composition canhave very different quality attributes if their constituents are organized differently. For example, a carton of ice cream taken from a refrigerator has a pleasant appearance andgood taste, but if it is allowed to melt and then is placed back in the refrigerator itsappea ra nce a nd t ext ur e cha nge dr a ma t i ca ll y a nd it woul d not be ac cept a bl e t o a consumer. Thus, there has been an adverse influence on its quality, even though itschemical composition is unchanged, because of an alteration in the structuralorganization of the constituents caused by the melting of ice and fat crystals. Another familiar example is the change in egg white from a transparent viscous liquid to anoptically opaque gel when it is heated in boiling water for a few minutes. Again thereis no change in the chemical composition of the food, but its physiochemical propertieshave changed dramatically because of an alteration in the structural organization of theconstituents caused by protein unfolding and gelation.The structure of a food can be examined at a number of different levels: Molecular structure ( 1 100 nm) . Ultimately, the overallphysicochemical properties of a food depend on the type of molecules present, their t hr ee- di me ns io na l s t ruct ur e a nd t heir i nt er a ct i ons wit h ea c h ot her. It is t her efor eimportant for food scientists to have analytical techniques to examine the structure andinteractions of individual food molecules. Microscopic structure ( 10 nm 100 m) . The microscopic structureof a food can be observed by microscopy (but not by the unaided eye) and consists of r egi ons i n a mat er ia l wher e t he mol ecul es a ss ocia t e t o for m di s cr et e p has es , e.g., emulsion droplets, fat crystals, protein aggregates and small air cells.

Macroscopic structure ( > 100m).

This is the structure that can beobs er ve d by t he una i d ed hu ma n e ye, e.g.,s u gar gr a nul es , la r ge a ir cel ls, r ais ons, chocolate chips. T he f or goi ng di s c us s i on ha s hi ghl i gh t e d a nu mb er of di ff er ent le vel s o f structure that are important in foods. All of these different levels of structure contributeto the overall properties of foods, such as texture, appearance, stability and taste. Ino r d e r t o d e s i g n n e w f o o d s , o r t o i m p r o v e t h e p r o p e r t i e s o f e x i s t i n g f o o d s , i t i s extremely useful to understand the relationship between the structural properties of foods and their bulk properties. Analytical techniques are therefore needed tocharacterize these different levels of structure. A number of the most important of these techniques are considered in this course. 1.2.3. Physicochemical Properties The physiochemical properties of foods (rheological, optical, stability,flavor) ultimately determine their perceived quality, sensory attributes and behavior during production, storage and consumption.