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1. JNTUH UNIVERSITY COLLEGE OF ENGINEERING,SCIENCE & TECHNOLOGY HYDERABAD SUBJECT: PHARMACEUTICAL FOOD ANALYSIS Topic: Analytical Methods For Ice Cream And Milk Powder PRESENTED BY PEDAPUDI DIVYA JYOTHI (23011S0404) UNDER THE GUIDANCE OF DR. R. APARANJITHA

2. MILK PRODUCTS ICE CREAM

3. INTRODUCTION • Ice cream is a frozen blend of a sweetened cream mixture and air with added flavourings. • It is usually made from dairy products such as milk  and cream combined with fruits or other ingredients andflavours. • It is sweetened with sugar or sugar substitutes. • The mixture is stirred to incorporate air spaces. • The result is smooth ,semi-solid foam that is solid at very low temperature (<2 ° C or 35 ° F ) 3                                                                                                                                                                                                           INTRODUCTION Ice cream is a frozen blend of a sweetened cream mixture and air with added flavourings . It is usually made from dairy products such as milk and Cream combined with fruits or other ingredients and flavours . It is sweetened with sugar or sugar substitutes. The mixture is stirred to incorporate air spaces. The result is smooth ,semi-solid foam that is solid at very low temperature (<2 ° C or 35 ° F)

4. Components % Composition Milk Fat > 10% - 16% Sucrose 9% - 12% Corn Syrup Solid 10%-14% Stabilizers 4%-5% Emulsifiers 0%-0.25% Water 55%-64% COMPOSITION :

5. ANALYSIS OF ICE-CREAM Preparation of sample Determination of Fat Determination of Protein Titrable Acidity Determination of Total Solids

6. PREPARATION OF SAMPLE OF ICE CREAM For samples taken in small packages, remove the packaging and place the sample in a clean, dry container fitted with an airtight closure. For samples taken from bulk or from large packages, keep them in their sampling containers.

7. DETERMINATION OF FAT PERCENT :- FAT : It provides structure, delivers flavour , boosts the creaminess and stabilises the tiny air bubbles that influence the creaminess. Either dairy fats or vegetable fat can be used such as cream, butter or butter oil. METHOD: Accurately weigh 4-5 g of the thoroughly mixed sample directly into fat extraction flask or Mojonnier tube, using free flowing pipette, dilute with water to approximately 10 ml, and mix by shaking. Add 2 ml ammonia; mix thoroughly, heat in water bath for 20 min at 60°C with occasional shaking, cool and then add ethyl alcohol. Extract the fat with diethyl ether and petroleum ether. Identify the clear extracted fat. Gerber Butyrometer

8. DETERMINATION OF PROTEIN:- Take 10 gm of the sample accurately weighted in a conical flask (it is convenient to weigh by difference). Add 50 ml distilled water to it.Add I ml. of phenolphthalein indicator solution to it followed by 0.4 ml saturated potassium oxalate solution. mix the contents of the flask and set it aside for 2min. Neutralize the contents of the flask with standard 0.1 NaOH solution to a pink coloured end point. Add 2 ml neutralized formaldehyde and again titrate with standard NaOH solution to the same pink shade. Note the volume of NaOH solution used (V). Calculation: Protein %.= V X 1.7

9. Dye Binding Method : One of the methods commonly used to determine the protein content in ice cream is the dye-binding method. This method involves using a specific dye that binds to the proteins present in the ice cream. The intensity of color formation, proportional to the protein present, is then measured. This method is relatively quick and easy to perform, making it a popular choice for protein analysis. The dye binding method has been found to correlate well with the Kjeldahl method, which is another widely used method for protein determination

10. Role Of Proteins In Ice Cream: Ice cream is not just a delicious treat; it also contains important proteins that play a vital role in its structure and characteristics. These proteins contribute to three main functional roles in the development of ice cream: emulsification, aeration, and solution properties. Emulsification Proteins form a protective layer around the fat droplets, allowing them to disperse evenly throughout the mixture. This emulsification process is crucial for achieving a rich and creamy mouthfeel in ice cream. Aeration proteins help to stabilize the air bubbles, preventing them from collapsing and maintaining a consistent structure. This aeration process gives ice cream a desirable texture and makes it enjoyable. Solution Properties They interact with other components in the mixture, such as sugars and minerals, influencing the overall viscosity and texture of the ice cream. This interaction also affects ice cream’s freezing and melting properties, ensuring that it remains stable throughout storage and consumption.

11. DETERMINATION OF TITRABLE ACIDITY:- Weight accurately about 10gm (weight by difference) of the sample into a 100ml flask. Add 50ml. of boiled and cooled distilled water to it. Mix properly. Add 1ml. Phenolphthalein indicator solution and titrate against standard sodium hydroxide solution 0.1N to a light pink colour end point. Note the volume of NaOH solution used and calculate the titratable acidity as follows. Titratable Acidity (as Lactic acid) % by weight = 9NV/w Where, N = Normality of the standard NaOH solution. V = Volume of the standard NaOH solution. W = Weight of the sample taken.

12. DETERMINATION OF TOTAL SOLID:- Weigh accurately clean and dry metal dish (dried & cool in a desiccator).Take about 2 gm of sample in it and weigh it again. Add 2-3 ml of distilled water to it, spread the sample properly in the dish and dry it on a hot plate carefully. Transfer the dish in a well-ventilated hot air oven at 100±1°C for one and a half hour. Transfer the dish in a desiccator for cooling and then weigh again Total solids % by weight = 100 x w3-wl Where wl-w2 WI= Weight of empty dish W2=Weight of dish with sample (before drying) W3Weight of dish with sample (after drying)

13. ADULTERANTS ADDED IN ICE CREAM : Low quality, cheaper and unhealthy (rather more harmful) sweeteners like Corn syrup, high fructose corn syrup, glucose syrups, etc.  Unhealthy gums added to increase the thickness of ice cream, impart a creamy texture, delay melting time due to added stickiness, and increased shelf life Not only these but pepperonil , ethylacetate , butraldehyde , emil acetate, nitrate, washing powder  etc are used Pepperonil is used as pesticide Etnyl acetate causes diseases affecting lungs kidneys hearts

14. MILK POWDER

15. Powdered milk, also known as dry milk or milk powder, is a dairy product that has been evaporated to remove most of the water content, resulting in a dry, powdery substance. The remaining particles are then collected, resulting in the formation of fine powder. One purpose of drying milk is to preserve it; milk powder has a far longer shelf life  than liquid milk and does not need to be refrigerated, due to its low moisture content. Another purpose is to reduce its bulk for the economy of transportation. Powdered milk and dairy products include such items as dry whole milk, nonfat (skimmed) dry milk, dry buttermilk, dry whey products and dry dairy blends.  It is derived from regular liquid milk through a process called spray drying, where the milk is heated and then sprayed into hot air, causing the to evaporate rapidly.

16. ANALYSIS OF MILK POWDER Preparation of sample Determination of moisture Determination of titrable acidity Determination of ash content Determination of sorched particle Determination of bulk density Determination of fat percent Determination of carbohydrates

17. PREPARATION OF SAMPLE Make homogeneous either by mixing or shaking or alternately rolling and inverting container. Avoid excessive temperature and humidity when opening sample container to prevent absorption of moisture

18. DETERMINATION OF MOISTURE IN DRIED MILK The sample is dried to constant weight at 102+2°c and the loss in weight reported as moisture Moisture% by mass =100 (m1-m2) (m1-m) Where M=mass in gm of the empty dish M1=initial mass in gm of the dish and lid with the material taken for analysis M2=final mass in gm of the dish and lid with the material after drying

19. DETERMINATION OF TITRABLE ACIDITY :- Take 10ml of sample and 10 ml of distilled water in conical flask. Add I ml phenolphthalein indicator. Titrate with 0.1N NaOH solution Faint pink colour shows end point Indicates presence of lactic acid in milk Calculation:- %acidity :-volume of NaOH used x 0.09

20. DETERMINATION OF ASH CONTENT: 1. Ignite a porcelain crucible. 2. Cool the crucible till room temperature and weigh. 3. Weigh out 1-5 g of sample, and transfer to the pre-ignited crucible. 4. Heat up the sample carefully with a bunsen burner until all is calcined. Avoid that the product catches fire as some of the material may burn off. 5. Put the sample into the heating furnace overnight at 525°C, or until it is carbon-free.

21. 6. Cool in desiccator and weigh. Do not put too many crucibles in one desiccator as it will prolong the cooling time. 7. All measurements are to be made in duplicate Result a-b % ash = —— × 100 c-b a = weight of crucible + dry sample b = weight of crucible c = weight of sample and crucible Two determinations must not differ more than 5 % relative. Specify temperature and time with each result.

22. DETERMINATION OF FAT PERCENT :- . Weigh accurately 1-2 g of prepared sample in a 100 ml beaker. Add 10 ml of conc. hydrochloric acid. Heat on a Bunsen burner, stirring continuously with a glass rod, or on a boiling water bath until all solid particles are dissolved. Cool to room temperature. Add 10 ml of ethyl alcohol first to the beaker and later transfer the contents to the Mojonnier fat extraction flask.

23. Liberated fat is extracted with alcohol, ethyl ether and petroleum ether. Ethers are evaporated and residue left behind is weighed to calculate the fat content. Fat % (w/w) = 100 x (W1-W2) W Where W1 = Weight in g of contents in the flask or metal dish or glass bowl before removal of fat. W₂ = Weight in g of contents in the flask or metal dish or glass bowl after removal of fat W = Weight in g of material taken for the test.

24. DETERMINATION OF BULK DENSITY : - Weight 30 gm of powder in 100 ml cylinder. Fix the cylinder in the frame of bulk density apparatus. Fix the apparatus for thirty strokes. Switch on the apparatus. The apparatus will take 30 strokes. Note the volume of the powder in the cylinder. Calculate the density as follows: Density = mass volume Mass = Weight of the Powder Volume = Volume of powder after 30 strokes.

25. DETERMINATION OF SORCHED PARTICLES:- Take 10 grams of SMP or 13 grams of WMP into 100 ml of distilled water in a flask. Observe the bottom of the flask in which powder is reconstituted after keeping undisturbed for some time. Filter the reconstituted milk through scorched particle tester and compare the filter pad with ADPI comparison card. Powder with scorched particles more than Disk B reading is rejected.

26. DETERMINATION OF TOTAL CARBOHYDRATES Total carbohydrates can be determined adding the mass of moisture, fat, protein and ash content and deducting it from 100 to give carbohydrate content by difference. Total carbohydrate including sucrose, dextrose and dextrins , maltose or lactose percent by weight = 100- (A+B+C+D) Where A Percent by mass of moisture B = Percent by mass of total protein. C= Percent by mass of fat D = Percent by mass of Total ash

27. Moisture Content The moisture content in milk powder affects its shelf life and reconstitution properties. It can be determined by drying the milk powder in an oven. Protein Content The protein content in milk powder is a key parameter that affects its nutritional value and functional properties. It can be determined by the Kjeldahl method. Fat Content The fat content in milk powder affects its flavour , texture and functionality. It can be determined by the Gerber method or the Soxhlet method. Ash Content The ash content in milk powder is an indicator of mineral content and can be determined by incineration of the milk powder.

28. ADULTERATIONS USED IN MILK POWDER : Urea Detergents Ammonium sulphate Boric acid Calk powder caustic soda Benzoic acid Salicylic acid Hydrogen peroxide Sugars and melamine

29. DETECTION OF ADDED UREA IN MILK POWDER Procedure-: 5ml milk+5ml 1.6% of p-dimethyl amino benzaldehyde(DMAB) distinct yellow colour observed in milk The control(Normal milk) shows a slight yellow colour due to presence of natural urea.

30. DETECTION OF CANE SUGAR IN MILK POWDER Principle:-Fructose + Resorcinol in HCL→ Red colour Procedure-: Milk powder + Conc HCL Filter-- 1 ml filtered milk powder serum & 5 ml modified resorcinol-HCL reagent after this withdraw the tube & observe the colour

31. Thank you