ExFLP-16 Determination of Magnetic Metal Particles and Heavy Filth in Chocolate and Cocoa

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2902B885DFFC4FC993C4E9BFDEA9BE08

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2012-3-3

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Published on the Food Directorate’s (Health Canada's) website at http://www.hc-sc.gc.ca/food-aliment.,Government of Canada Gouvernement du Canada,Laboratory Procedure ExFLP-16,September 1997,HEALTH PRODUCTS AND FOOD BRANCH,OTTAWA,DETERMINATION OF MAGNETIC METAL PARTICLES AND HEAVY,FILTH IN CHOCOLATE AND COCOA,Research Division, Bureau of Microbial Hazards,Food Directorate, Postal Locator: 2204A2,Health Canada, Ottawa ON K1A 0L2,1. APPLICATION,This method is applicable to the sampling and examination of chocolate and cocoa for magnetic metal particles,and heavy filth to determine compliance with Sections 4, 5 and 7 of the Food and Drugs Act.,2. DEFINITION OF TERMS,A lot is defined as that amount (volume, weight, etc.) of the food which is produced, stored and/or shipped under,conditions as nearly uniform as possible, preferably designated by a common container code or marking, and, in,any event, consisting of not more than one variety, grade or type of product from a single identifiable source.,3. SAMPLING,3.1 Scrutinize the entire lot for live infestation. If live infestation is found, do not sample until after fumigation,or other effective treatment.,3.2 Obtain three sample units selected at random from the lot of at least 100 g each for chocolate and at least,50 g each for cocoa using appropriate sampling equipment and containers. Three sample units constitute,a sample.,3.3 Each sample unit must be kept separate and labelled 1, 2 and 3. Complete information respecting the lot,size, weight of individual containers, country of origin, exporter, importer, or domestic manufacturer, and,product and lot identification should be recorded and should accompany the sample.,4. MATERIALS AND SPECIAL EQUIPMENT,1) Stirrer hot plate,2) Smooth spin bar magnets, teflon coated (1 x 5 cm recommended),3) Non-magnetic tweezers,4) Glass beakers (0.6 - 1.0 L) and suitably sized covers,5) Glass or plastic stirring rod,6) Wash bottles,- 2 - ExFLP-16,September 1997,7) Strong magnet,8) Suction filtration apparatus with Buchner or Hirsch funnel,9) Ruled filter paper (filter paper should be larger than funnel),10) Ashless filter paper (filter paper should be larger than funnel),11) Chloroform or trichloroethylene,12) 1N HCl,13) Ethanol (95%),14) 1% sodium lauryl sulphate solution (detergent),15) Filtered or distilled water,16) Petri dishes,17) Cellotape,18) Acetone,19) Fine, non-magnetic probe (platinum or glass recommended),20) Glycerol - alcohol (95%) mixture (1:1),21) Stereoscopic microscope (10-30x),22) Platinum crucible,23) Muffle oven,24) Desiccator,5. PROCEDURE,The examination shall be carried out in accordance with the following instructions.,5.1 Preparation of Analytical Units,5.1.1 In a random fashion from a sample unit of chocolate, weight 100 g. This 100 g constitutes an analytical,unit.,5.1.2 In a random fashion from a sample unit, weigh 50 g cocoa. This 50 g constitutes an analytical unit.,5.1.3 Repeat Step 5.1.1 or 5.1.2 for remaining two sample units.,5.2 Isolation - Magnetic Metal Particles,- 3 - ExFLP-16,September 1997,NOTE: Because of the fragility and rapid oxidation of metal particles, it is suggested that Steps 5.2.1 to 5.2.3,be performed without interruption.,5.2.1 Transfer an analytical unit to a beaker.,5.2.2 Add 250 ml of cholorform or trichloroethylene. Cover and mix with a glass or plastic rod until a,homogeneous suspension is obtained, using heat if necessary.,5.2.3 Wash a magnetic stirring bar with 1N HCl to ensure that the bar is free of metal particles. Rinse bar with,water until free of acid and dry.,5.2.4 Drop the magnetic stirring bar into beaker containing chocolate or cocoa suspension, cover and place on,stirrer hot plate.,5.2.5 Set to low heat and stir suspension for 10 minutes.,5.2.6 Shut off stirrer and remove beaker from hot plate. Lift magnet out of suspension using a second magnet,on the outside of the beaker. Remove magnetic stirring bar with non-magnetic tweezers.,5.2.7 Using wash bottles, rinse magnetic particles from stirring bar into a second beaker, first with small amounts,of chloroform, then with ethanol and then with large amounts of detergent until the particles are washed,off. Finally rinse stirring bar with ethanol. Add 20-25 ml of chloroform to the washings to dislodge particles,that adhere to the beaker.,5.2.8 Return stirring bar to chocolate or cocoa suspension, cover and place on stirrer hot plate.,5.2.9 Repeat stirring and washing two more times, transferring each washing into a separate beaker.,5.2.10 Filter each washing through separate labelled ruled filter papers using suction filtration apparatus.,5.2.11 To ensure that small particles, ……

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