LAB. MANUAL 1 - FSSAI

1 LAB. MANUAL 1 MANUAL OF METHODS OF ANALYSIS OF FOODS FOOD SAFETY AND STANDARDS AUTHORITY OF INDIA MINISTRY OF HEALTH AND FAMILY WELFARE GOVERNMENT OF INDIA NEW DELHI 2015 MILK AND MILK PRODUCTS ACKNOWLEDGEMENT Deepest Sense of Gratitude and Indebtedness to all the Members of the Panel Method of Sampling and Analysis and Experts, who have helped, supported knowledge and insight, have led the successful completion of Revision of manuals. Sincere Thanks to the Panel, Chairman for his valuable guidance, and encouragement and the Secretariat of this panel who have worked hard throughout the tenure of revision work. Deepest Appreciation to the Chairperson, FSSAI and CEO, FSSAI for the cooperation, support and constant encouragement, without which the work would not have seen the light of day.

2 ** MILK AND MILK PRODUCTS 2015 1 MANUAL FOR ANALYSIS OF MILK AND MILK PRODUCTS TABLE OF CONTENTS TITLE PAGE NO. 1 liquid MILK 7 Preparation of Sample of Milk 7 Detection of Adulterants in Milk 7 Detection and Quantification of Cane Sugar 7 Detection and Quantification of Starch in Milk 9 Detection of Cellulose in Milk 10 Detection of Added Urea in Milk 11 Detection of Ammonium Compounds in Milk 13 Tests for Presence of Sulphates in Milk 14 Detection and Estimation of Added Glucose in Milk 15 Detection of Sodium Chloride in milk 17 Detection of Presence of Foreign Fat in Milk 17 Detection of Nitrates (Pond Water) in Milk 19 Detection of Neutralizers in Milk 20 Detection of Hypochlorites and Chloramines in Milk 21 Test for Quaternary Ammonium Compounds in Milk 23 Test for Presence of Anionic Detergent in Milk 24 Test for Presence of Skimmed milk Powder in Natural milk (Cow, buffalo, goat, sheep)

3 25 Test for Detection of Gelatine in Milk 26 Test for Presence of Formalin in Milk 27 Test for Presence of Hydrogen Peroxide in Milk 28 Test for Presence of Boric acid and Borates 29 Test for Presence of Salicylic acid in Milk 30 Other Tests for Chemical Analysis of milk 31 Alkaline Phosphatase Test for Checking Efficiency of Pasteurisation in liquid Milk 31 Turbidity Test for Checking Efficiency of Sterilization in liquid Milk 33 determination of Total Solids (Gravimetric method) 34 MILK AND MILK PRODUCTS 2015 2 TITLE PAGE NO. determination of Fat in Milk 36 Method 1. Gerber Method 36 Method 2. Rose-Gottlieb Method 39 Method 3. Acid Digestion Method (Werner Schmidt Method) 41 2 CREAM, INCLUDING STERILISED CREAM, WHIPPED CREAM AND MALAI 43 Preparation of Sample of Cream 43 determination of Fat in Cream 43 Method 1.

4 Rose Gottlieb Method. 43 Method 2. Werner Schmidt Method 44 Detection of Presence of Thickeners in Cream 44 Method 1. for Detection of Starch in Cream 44 Method 2. for Detection of Gelatine in Cream 44 3 CREAM POWDER 45 Preparation of Sample of Cream Powder 45 determination of Moisture in Cream Powder 45 determination of Fat Content in Cream Powder 46 determination of Milk Protein in Milk Solids not Fat of Cream Powder 46 Method 1. As per AOAC Method 47 Method 2. determination of Protein Content Using IDF Procedure 48 4 CURD OR DAHI 49 Preparation of Sample of Dahi 49 determination of Fat in Dahi 49 Test for the Presence of Starch in Dahi 49 determination of Total Solids in Dahi 49 Method 1. Sodium Hydroxide Method 49 Method 2. Zinc oxide Method 50 determination of Total Solids in Dahi Sweetened with Cane Sugar 53 5 CHHANNA OR PANEER 54 Preparation of Sample of Channa/Paneer 54 determination of Moisture in Channa/Paneer 54 MILK AND MILK PRODUCTS 2015 3 TITLE PAGE NO.

5 determination of Fat (by Acid Digestion Method) in Channa/Paneer 56 Detection of Starch in Channa 56 6 CHEESE (ALL VARIETIES) 57 Preparation of Sample of Cheese 57 determination of Moisture in Cheese 57 determination of Milk Fat (by Acid Digestion Method) in Cheese 57 7 ICE CREAM, SOFTY ICE CREAM, CHOCOLATE ICE CREAM, KULFI, MILK ICES OR MILK LOLLIES AND FROZEN DESSERT / CONFECTION 58 Preparation of Sample of Ice Cream 58 determination of Total Solids in the Ice cream 59 determination of Weight per Unit Volume or Over-run in Ice Cream 59 determination of Fat in Ice-Cream (Rose-Gottlieb method) 61 determination of Protein (Kjeldahl method) in Ice-Cream 61 Method 1. As per DGHS MANUAL (2005) 61 Method 2. determination of Protein Content using IDF Procedure 63 determination of Added Starch in Ice Cream 63 8 DRIED ICE CREAM MIX / DRIED FROZEN DESSERT / CONFECTION 65 Preparation of Sample of Dried Ice Cream Mix 65 determination of Moisture Content in Dried Ice Cream Mix 65 9 CONDENSED / EVAPORATED (SWEETENED, UNSWEETENED AND SKIMMED) MILK 66 Preparation of Sample of Condensed/Evaporated Milk 66 determination of Total Solids in Condensed/Evaporated Milk 66 determination of Fat by Rose-Gottlieb's Method in Condensed/Evaporated Milk 68 determination of Sucrose Content in Condensed/Evaporated Milk 69 Lane-Eynon (Volumetric)

6 Method 69 Polarimetric Method for determination of Sucrose in Condensed Milk 77 determination of Titratable Acidity in Condensed/Evaporated Milk 82 determination of Milk Protein in Milk Solids not Fat of Condensed/Evaporated Milk 83 MILK AND MILK PRODUCTS 2015 4 TITLE PAGE NO. 10 MILK POWDER (WHOLE, SKIMMED, PARTIALLY SKIMMED) INFANT MILK FOOD, INFANT FORMULA, MILK CEREAL WEANING FOOD, PROCESSED CEREAL BASED WEANING FOOD 84 Preparation of Sample of Dried Milk 84 determination of Moisture in Dried Milk 84 determination of Fat in Dried Milk 86 determination of Titratable Acidity in Dried Milk 86 determination of Total Carbohydrates in Dried Milk 87 determination of Milk Protein in Milk Solids not Fat of Dried Milk 88 determination of Total Ash on Dry Basis in Dried Milk 88 determination of Ash Insoluble in Hydrochloric Acid (for Infant Foods and Processed Cereal based Weaning Foods) 89 determination of Crude fibre (in Processed Cereal Weaning Foods)

7 91 determination of the Solubility Index in Milk Powder 92 determination of the Solubility Percent in Milk Powder 94 11 KHOA 96 Preparation of Sample of Khoa 96 determination of Moisture in Khoa 96 determination of Fat content in Khoa 96 determination of Starch in Khoa 97 Detection of sucrose in Khoa 97 12 TABLE (CREAMERY), AND DESHI BUTTER 99 Preparation of Sample of Butter 99 determination of Moisture in Butter 99 determination of Fat and Curd (Milk solids not Fat) in Butter 100 determination of Salt Content in Butter 102 Method 1. (Volhard's Method) 102 Method 2. (Mohr's Method) 104 13 GHEE / BUTTER FAT /BUTTER OIL AND ANHYDROUS MILK FAT / ANHYDROUS BUTTER OIL 107 Preparation of Sample of Ghee 107 determination of Moisture in Ghee 107 determination of Butyro Refractometer Reading in Ghee 108 determination of Free Fatty Acids in Ghee 113 determination of Reichert-Meissel and Polenske Value in Ghee 115 Test for Detection of Vanaspati in Ghee (Boudouins Test) 122 Detection of Vegetable Fat in Ghee 123 MILK AND MILK PRODUCTS 2015 5 TITLE PAGE NO.

8 determination of Peroxide Value in Ghee 123 14 CHAKKA AND SHRIKHAND 126 Preparation of Sample 126 determination of Milk Solids 126 determination of Fat 126 determination of Protein 126 determination of Titratable Acidity 126 determination of Total Ash 126 determination of Sucrose Content 126 15 YOGHURT 127 Preparation of Sample of Yoghurt 127 determination of Milk Solids not Fat in Yoghurt 127 determination of Milk Fat in Yoghurt 127 determination of Protein Content in Yoghurt 127 determination of Titratable Acidity in Yoghurt 128 16 WHEY POWDER 129 Preparation of Sample of Whey Powder 129 determination of Moisture in Whey Powder 129 determination of Fat in Whey Powder 129 determination of Milk Protein in Whey Powder 129 determination of Total Ash in Whey Powder 129 determination of pH in Whey Powder 129 determination of Lactose in Whey Powder 129 17 EDIBLE CASEIN PRODUCTS 131 Preparation of Sample of Casein/Caseinates 131 determination of Moisture in Casein/Caseinates 131 determination of Fat in Casein/Caseinates 131 determination of Milk Protein in Casein/Caseinates 135 determination of Casein in Protein in Casein/Caseinates 135 determination of Lactose Content in Caseins/Caseinates (by Photometric Method).

9 136 determination of Ash Content in Casein/Caseinates 139 determination of Fixed Ash (ash including P2O5) Content in in Casein/Caseinates 141 determination of Free Acidity in Caseins/Caseinates 143 determination of pH in Casein/Caseinates 145 18 determination OF LACTOSE BY COLORIMETRIC METHOD IN MILK BASED SWEETS 148 MILK AND MILK PRODUCTS 2015 6 TITLE PAGE NO. determination of Lactose by Colorimetric Method 148 determination of Lactose by high - performance liquid chromatography ( hplc ) 149 19 DETERMIANIOTN OF TOTAL NITROGEN CONTENT IN MILK/MILK PRODUCT BY KJELDAHL METHOD 157 determination of Total Nitrogen/Crude Protein in Milk 158 Method 1. Macro Kjeldahl Method (IDF 20B: 1993) 158 Method 2. Block Digestion/ Steam Distillation method (IDF 20B: 1993) 165 Method 3. Micro Kjeldahl Method 171 determination of Non-Protein Nitrogen (NPN) in Milk 175 determination of True Protein Nitrogen Content in Milk 178 determination of Protein content in milk and milk products by BIS method 181 20 determination OF MELAMINE AND CYANURIC ACID IN MILK, MILK PRODUCT AND INFANT FORMULAE GUIDELINES 183 Method 1.

10 Detection of Non-Protein Nitrogen (NPN) Containing Substances in Milk 184 Method 2. ELISA based Methods 185 Method 3. ISO Method 186 .. MILK AND MILK PRODUCTS 2015 7 1. liquid MILK Buffalo milk, cow milk, goat milk, sheep milk, mixed milk, standardised milk, full cream milk, recombined milk, toned milk, double toned milk, and skimmed milk as laid down under FSSAI Rules. Preparation of Sample of Milk Samples are received after few days of drawl and contain preservative ( formalin). Warm the sample to 37- 40 C by transferring it to the beaker and keeping it in a water bath maintained at 40 - 45 C. Stir slowly for proper homogenisation. Mix sample thoroughly by pouring back into the bottle, mixing to dislodge any residual fat sticking to the sides and pour it back in the beaker.