MILK ANALYTICAL

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Milk Quality Adulterants and Contaminants in Milk Physicochemical Properties of Milk and their Importance Milk Quality Evaluation/Analysis Parameters for Milk Analysis Platform Testing

³It is not possible to produce good quality market milk and milk products from bad quality raw milk.´

Milk Quality Any company works for profit which is measured in terms of money earned by company. This success is indicated by 'repeat buys' of the product-means consumer's satisfaction-a measure goal of a manufacturer. In order to increase 'repeat buys' the manufacturer must identify consumers requirements in terms of characteristics or attributes of the product. This combination of attributes/characteristics that contribute to the acceptability of the product , is defined as 'Quality'. Quality of a product/milk is the sum of the following kind of attributes. Ø Physico-chemical attributes-nutritive elements, pH, acidity, Boiling point, freezing point etc. Ø Microbiological attributes-spoilage causing or pathogenic/toxin producing microorganisms. Ø Sensory attributes-colour, texture, odour, taste

Adulterants and Contaminants

ADULTERANTS are Substances, addition of which makes the food poorer in quality. CONTAMINANTS are Dangerous or disease-carrying substances, addition of which makes the food impure. examples: Pesticides /Insecticides

arsenic) Aflatoxin. Microbiological analysis Parameters for Milk Analysis y y y y Lactometer reading Fat Total solids SNF . aroma etc. parasiticus Physical contaminants. Physicochemical Properties of milk Physical state Acidity & pH Density & specific gravity Colour Flavour Viscosity Surface tension Refractive index Specific heat Electrical conductivity Oxidation-reduction potential Boiling point Freezing point Importance of properties: Ø Ø Ø Ø Helps in detection of adulteration. Helps in processing of milk & milk products. lactic acid %. plastics. dirt.from Aspergillus flavus & A. cadmium. stones.Antibiotics Industrial waste/ chemicals ± Heavy metals (lead. protein %. etc. specific gravity etc.metal fragments. Chemical analysis ± fat %. insects & others. glass. Physical analysis ± boiling point. Helps in determining quality of milk. Helps in evaluating physical changes in milk & milk products during processing Quality Evaluation/Analysis Organoleptic / Sensory analysis ± taste. flavour. mercury.

This chamber causes the instrument to float. calcium. Inside the lactometer there may be a thermometer extending from the bulb up into the upper part of the stem where the scale is located. Remove and read fat content in % Total solids: (milk constituents excluding water) .33g) of milk 3. Centrifugation ( 5 min. Amyl alcohol. as the fat globules soon rise and there fore the lower part of the lactometer would be resting in partially skimmed milk. with the graduation ranging from 15 at the top to 45 at the bottom. then the lactometer is inserted as soon as the instrument comes to the rest . The addition of water in milk result in the lowering of lactometer reading. Milk Fat Methods Babcock method Gerber method Roese-Gottlieb method Gerber Method: Materials: Butyrometer. citric acid. Each division is known as the lactometer degree. animal (tissue) or vegetable fat. ash Adulterants and Contaminants :Dirt. sample of the milk is thoroughly mixed. This thermometer does not record temperature above 380C thus this liquid does not put into the milk above this temperature. Gerber centrifuge. Reading the lactometer: In taking the lactometer reading of milk. Insert stopper 5. Note the temp of the milk when reading the lactometer and correct the lactometer degrees to standard temperature. and pour the milk into a glass measuring cylinder which is large enough to float the lactometer freely. Take 10ml of Sulphuric acid(sp. Lactometer: Lactometer consists of a long cylinder stem connected to the body. Add 1 ml amyl of alcohol 4.gravity 1. copper. urea. attached to the lower end of the body is the bulb which is filled with mercury to cause the lactometer to sink up to the proper level and to float in and up right position in the milk.read the division at the top of the meniscus film and on a level with the milk. added dyes. preservatives. which is a large air chamber. The reading should be taken with a little delay as possible. antibiotics and others Methyl blue test and bacteriological examination Lactometer reading is required to determine the per cent water or solids present in milk. Sulphuric acid. The average reading of normal whale milk is 32. can sugar. Hence this test is applied to detect the adulteration of milk with water. lactose. Invert & shake 6.y y y y Lact ometer reading Efficiency of pasteurization Protein. in Gerber Centrifuge) 7. starch. Standard pipette for milk Procedure: 1. Add 11 ml (11. Just below the thermometer is the lactometer scale. chloride. lactic acid. detergents.82) in butyrometer 2.

14 4 TS= LR= F = % Total solids Lactometer reading % Fat Solids Not Fat (SNF): (milk constituents excluding fat and water) % SNF = % TS . It is filtered. y After making up the volume to 100 ml with distilled water. .% Fat Lactose Method I Modified Lane & Eynon Method. standard solution of lactose (2. 20 ml milk.7 % barium hydroxide solution slowly with agitation followed by 20 ml of zinc sulphate solution.Hehner and Richmond formula LR( at 60 0F) X 0.29 TS= ------------------------. Method II y In 100 ml volumetric flask.2 F + 0. mg of invert sugar represents thefactor for Fehling's solution.+1. y The supernatant thus obtained is used to determine lactose content by titrating against Fehling solution using methylene blue as indicator. Ranganna.5 mg/ml)is used to determine factor for Fehling's solution. 1986 y 10 gm of the sample is deproteinized by adding 20ml of 2. The lactose content in the sample is calculated according to the following expression % lactose = [(mg of invert sugar x dilution )/(titre value x wt of sample) x 1000] where. y The contents are allowed to stand for 10min and than transffered to 100ml volumetric flask.12 ml 10% sodium tungstate and 15 ml 2/3 N H2SO4 are added and make upto 100 ml with water. the contents are filtered through watman # 4 filter paper.

1 N NaOH to end point. Protein = Total N x 6.5 .2 g CuSO4. % Chloride = (15 -TV ) x 0.01 % Chloride = (% Chlorine x 58. Protein % = V x 1. Titrate the excess acid against 0.Casein = Whey Proteins Kjeldahl Method y y y y y y Add 10 g milk. % Lactose = (0.0291 N) solution is added to 10 ml milk. Distill the contents in Kjeldahl distillation apparatus after adding 50% NaOH until it gives pink colour with phenolphthalein. Dilute it with 200 ml distilled water. y Titrate the same to end point with 0.and 10 g potassium oxalate to the Kjeldahl flask.) Protein & Casein Estimation Formal Titration Method y Pipette out 10ml of milk into a 100 ml flask.1 N H2SO4.1 N NaOH.067 X 100 X 100)/(TV X 20 X sp.1 N NaOH using methyl red indicator. y Titrate the milk against 0. y Add 2 ml of neutral formalin and mix well. Heat the flask for 2-3 hrs. 0. Volume of NaOH in second titration is V. gr.38 Protein .38 Chloride Estimation y y 15 ml of Silver nitrate (0.0014 x 100)/ wt of sample. 25 ml H2SO4. y Add 0.7 Casein % = V x 1. Distill ammonia in 50 ml 0.0291 N ). Total N = (TV x 0. y Add 5 drops of Phenolphthalein indicator. Titrate it with Potassium thiocynate ( 0.45 )/35.4 ml of saturated potassium oxalate solution and keep it aside for 2-4 min without disturbing.y The filtrate is titrated with 25 ml benedict's solution until it changes to white colour.

Enzyme has the ability to liberate phenol from phenol phosphoric acid compounds. Free phenol gives a deep blue colour with certain organic compounds. Colour intensity is measured by colourimetry. If the milk is under pasteurized it gives positive reaction to phosphatase test.Efficiency of pasteurization measured by Alkaline phosphatase test Alkaline phophatase is an enzyme present in raw milk.13-0. Blue colour indicates improper pasteurization DSPP ---.alkaline phophatase------> free phenol (phenol phosphoric acid compound) + ------->indophenol(blue colour) 2.14 % Buffalo milk---0. Milk Acidity Natural or Apparent Acidity Due to presence of already present natural constituents like casein. Developed Acidity or Real acidity Due to lactic acid.14-0. This enzyme is heat labile and destroyed by adequate pasteurization. CO2etc. Disodium phenyl phosphate is used as the source of phenol and 2.15 % Titratable Acidity Produced Lactic acid contributes a major part of the milk acidity and it can be measured by simple titration method. Determination of Titratable Acidity Apparatus: White porcelain dish . Milk is incubated with the DSPP and then indicator reagent is added. citrates. acid Phosphate. Action of them on lactose is responsible for lactic acid production in milk. formed as a result of growth of LAB in milk. It is expressed as per cent Lactic acid.6 DCQC (organic compound indicator reagent) Amount of phenol liberated is proportional to the active enzyme present. whey proteins. Cow milk------0. this is the basis for the phosphatase test.6 dichloroquinone ± chlorimide is the indicator reagent.

W=amount of milk taken for titration in gm. Titrate against 0. Add 0.1N Phenolphthalein indicator (1.5 ml /2-3 drops of phenolphalein indicator.0% solution in 95 % alcohol) Oxalic acid (for standardization of NaOH) Procedure: Measure accurately 10g/10ml of milk and take it into a porcelain dish/beaker. b) Lower fat percentage Higher density of milk Higher ratio of SNF: fat Detection of added water a.1 N NaOH till light pink colour appear for 10 seconds (time should not exceed 20 seconds). b.1 N NaOH required for titration. % TA= [( V X 0. Lower fat percentage .Pipette 10ml Burette Stirring rod Measuring cylinder Reagents: Standard NaOH---0.009)/W] 100 V= volume of 0. Milk Adultration Modes of adulteration: Removal of fat by skimming Addition of skim milk Addition of water Addition of starch and cane sugar for raising density Addition of neutralizers and other preservatives to increase keeping quality Procedure: a) Detection of skim milk a. Add equal volume of freshly boiled and cooled distilled water. c.

Add 0. 4. d) Detection of cane sugar Reagents: Resorcinol. 3.Take 3 ml milk in a test tube 2. Platform Testings include all those tests which are performed to check the quality of the incoming milk on the receiving platform. e) Detection of neutralizers Reagents: 1 per cent rosalic acid in alcohol. The rose red colour indicates the presence of carbonate. Acidity Purpose is to determine final acceptance or rejection of milk. so as to make a quick decision regarding its acceptance /rejection.b. The test tube is then placed in boiling water for 5 minutes 5. Take 1 ml milk in test tube. Add 1ml HCl 3.1g resorcinol and mix. Procedure: 1. concentrated HCl Procedure: 1. They are performed on each can /tanker of milk with the object of detecting milk of inferior or doubtful quality so as to prevent it to be mixed with high-grade milk. Sometimes the term µRapid platform test¶ is used to refer mainly to the organoleptic or sensory tests which take very little time to perform. Add a few drops of 1 percent rosalic acid and mix it. d. 2. Take 1 ml milk in test tube 2. c. 5. c) Lower density of milk Lower SNF percentage Depression in freezing point Detection of starch Reagent: 1% iodine solution Procedure: 1. Cool it and add a few drop of 1per cent iodine solution 4. . Boil the content 3. Alcohol. 4. Blue colour disappears when the sample is boiled. Appearance of red colour indicate the presence of red colour indicate the presence of cane sugar. Add 5 ml alcohol. Appearance of blue colour indicates the presence of starch.( on the basis of pre-determined level).

Dye-reduction test( MBR or Resazurin) To determine extent of bacterial contamination. Freezing point Fat/SNF Payment purpose . COB To determine heat stability. Alcohol-Alizarin To determine both heat stability & pH. indicates excess level of LA due to microbial activities. 5 ml milk-----boiling-----clotting. Milk + MB dye----( incubation at 370C)--------------Reduction time Colour changes from Blue to White If RT is more²less contamination and vice versa DMC To identify types of microorganisms present SPC Todetermine extent of bacterial contamination.APT To determine heat stability of milk. Lactometer reading To detect adultration with water.

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