MANUAL OF METHODS 
                                                                  OF 
                                             ANALYSIS OF FOODS 
                                           
                                          SPICES AND CONDIMENTS 
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                             
                               FOOD SAFETY AND STANDARDS AUTHORITY OF INDIA 
                                     MINISTRY OF HEALTH AND FAMILY WELFARE 
                                                    GOVERNMENT OF INDIA 
                                                             NEW DELHI  
                                                                 2016 
                                                                                          SPICES AND CONDIMENTS  2016 
                                            MANUAL FOR ANALYSIS OF SPICES AND CONDIMENTS 
                                                                      
                                                              TABLE OF CONTENTS 
                                                                                                                       
                             S.NO.                             TITLE/METHOD                                     PAGE NO. 
                                                                                                                     2 
                              1.0        Preparation of Sample 
                              2.0        Determination  of  Extraneous  Matter  and  other                           2 
                                         Refractions 
                              3.0        Determination of Moisture                                                   2 
                              4.0        Determination of Total Ash                                                 12 
                              5.0        Determination of Ash Insoluble in dilute HCl                               14 
                              6.0        Determination of Cold Water Extract                                        15 
                              7.0        Determination of Alcohol Soluble Extract                                   15 
                              8.0        Determination of Calcium Oxide                                             17 
                              9.0        Determination of Non Volatile Ether Extract                                18 
                              10.0       Determination of Volatile Oil                                              19 
                              11.0       Determination of Crude Fibre                                               22 
                              12.0       Determination of Allyl isothiocyanate in Mustard                           24 
                              13.0       Determination of p-hydroxybenzyl isothiocyanate in S.                      25 
                                         alba (White Mustard) 
                              14.0       Black Pepper                                                               26 
                              15.0       Saffron                                                                    30 
                              16.0       Turmeric Whole                                                             34 
                              17.0       Asafoetida                                                                 37 
                              18.0       Microscopic Examination of Spices                                          39 
                                                             
                              19.0       Detection of Argemone seeds in Mustard                                     40 
                              20.0       Detection of Mineral Oil in Black Pepper                                   40 
                              21.0       Detection of Papaya seeds in Black Pepper                                  41 
                              22.0       Detection of Turmeric in Chillies and Corriander                           42 
                              23.0       Detection of Oil Soluble Colour                                            42 
                              24.0       Determination of  Light  and  Heavy  Filth  in  Spices  and                42 
                                         Condiments 
                              25.0       Method for capsaicin content in chilli powder                              42 
                              26.0       Method for measuring colour value in chillies                              48 
                                         References                                                                 50 
                        Note:  The test methods given in the manuals are validated/ standardized test methods. 
                        However, it would be the responsibility of the respective testing laboratory to confirm that 
                        the  above  methods  are  validated  in  its  laboratory  and  gives  proper  result  in  their 
                        laboratory.     
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                                                                                                                                               SPICES AND CONDIMENTS  2016 
          
                                                     MANUAL FOR ANALYSIS OF SPICES AND CONDIMENTS 
                                              Spices  and  condiments  are  added  to  foods  in  small  amounts  but  they  make 
                              important contribution to the sensory qualities due to presence of volatile and fixed oils. 
                              Standards for Spices and Condiments are laid down under Food Safety and Standards 
                              (Food Products Standards and Food Additives) Regulations, 2011. 
                               
                              1.0  Preparation of sample 
                               
                                              Grind laboratory sample as quickly as possible in a grinding mill to pass sieve 
                              with 1 mm diameter aperture. Avoid undue heating of apparatus during grinding. Mix 
                              carefully to avoid stratification (layering). Store in a dry stoppered container. 
                               
                              (Ref: - IS Specification No IS 1797 – 1985 Methods of Test for Spices and Condiments/ 
                              AOAC 17th edn 2000, Official Method 920.164 Preparation of Test sample) 
                               
                              2.0  Determination  of  Extraneous  Matter  and  other  Refractions  in  Whole  spices              
                                        
                                              Thoroughly mix the sample and weigh 100 – 200 gm depending on the nature of 
                              the material (10 – 20 gm in case of small sized spices), note down the exact weight and 
                              spread in an enameled tray. Separate extraneous matter and other refractions by hand. 
                              Weigh each fraction and calculate percentage. 
                               
                              (Ref: - IS Specification No IS 1797 – 1985 Methods of Test for Spices and Condiments) 
                               
                              3.0   Determination of Moisture (Dean and Stark Toluene Distillation Method) 
                               
                              3.1 Principle 
                               
                                              The amount of water is determined by distilling the material with an organic 
                              liquid not miscible with water and collecting the distillate in a graduated tube. 
                               
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                                   SPICES AND CONDIMENTS  2016 
   
        3.2 Reagents 
         
           Toluene - Saturate with small quantity of water and distill. Use the distillate for 
        determination of moisture. 
         
        3.3 Apparatus  
         
           Moisture Distillation Apparatus - consists of a 500 mL short neck round bottomed 
        flask heated using a heating mantle and provided with a reflux condenser discharging into 
        a trap connected to the flask. The trap serves to collect and measure the condensed water 
        and to return the condensed solvent to the flask (See figures below) and a copper wire 
        long enough to extend throughout the condenser with one end twisted into a spiral. The 
        diameter of the spiral should be such that it fits snugly within the graduated portion of the 
        receiver and yet it can be moved up and down. 
         
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