1、BRITISH STANDARD BS 4585-14: 1983 ISO 1208:1982 Methods of test for Spices and condiments Part 14: Determination of filth UDC 633.82/.84:664.5:543.869BS4585-14:1983 This British Standard, having been prepared under the directionof the Food and Agriculture Standards Committee,was published underthe a
2、uthority of the BoardofBSI and comes intoeffecton 31May1983 BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference FAC/7 Draft for comment 81/54293 DC ISBN 0 580 13315 X Committees responsible for this British Standard This British Standard was published un
3、der the direction of the Food and Agriculture Standards Committee FAC/-. Its preparation was entrusted to Technical Committee FAC/7 upon which the following bodies were represented: Association of Public Analysts British Essence Manufacturers Association British Food Manufacturing Industries Researc
4、h Association Co-operative Union Department of Industry (Laboratory of the Government Chemist) Food Manufacturers Federation Incorporated General Produce Brokers Association of London Ministry of Agriculture, Fisheries and Food Overseas Development Administration Tropical Products Institute Amendmen
5、ts issued since publication Amd. No. Date of issue CommentsBS4585-14:1983 BSI 10-1999 i Contents Page Committees responsible Inside front cover National foreword ii 0 Introduction 1 1 Scope and field of application 1 2 Reference 1 3 Definition 1 4 Principle 1 5 Reagents 1 6 Apparatus 1 7 Sampling 2
6、8 Procedure 2 9 Expression of results 3 10 Test report 3 Annex Pancreatin Specification 5 Figure Wildman trap flask (6.1), showing method of use 4 Publications referred to Inside back coverBS4585-14:1983 ii BSI 10-1999 National foreword This Part of BS4585has been prepared under the direction of the
7、 Food and Agriculture Standards Committee, and is identical with ISO 1208:1982 “Spices and condiments Determination of filth”, prepared by Subcommittee 7, Spices and condiments, of Technical Committee ISO/TC 34, Agricultural food products, and published by the International Organization for Standard
8、ization (ISO). Terminology and conventions. The text of the International Standard has been approved as suitable for publication as a British Standard without deviation. Some terminology and certain conventions are not identical with those used in British Standards; attention is drawn especially to
9、the following. The comma has been used as a decimal marker. In British Standards it is current practice to use a full point on the baseline as the decimal marker. Wherever the words “International Standard” appear, referring to this standard, they should be read as “British Standard”. NOTETextual er
10、ror. In 8.1.1, line 2 “breaker” should be read as “beaker”. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from
11、legal obligations. Cross-reference International Standard Corresponding British Standard ISO 948:1980 BS 4540 Sampling of spices and condiments Part 1:1981 Methods of sampling (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 to 6, an
12、inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.BS4585-14:1983 BSI 10-1999 1 0 Introduction International Standards specifying requirements for sp
13、ices and condiments prescribe, inter alia, that spices and condiments shall be practically free from dead insects, insect fragments and rodent contamination. For testing compliance with this requirement, hand lens examination is adequate only in the case of whole spices and condiments. For ground sp
14、ices and condiments, the method to be used is that specified in this International Standard, especially in cases of dispute. The method is applicable to most spices and condiments. In view of the number and variety of such products, however, it may be necessary in particular cases to modify the meth
15、od or even to choose a more suitable method. Such modifications and other methods will be indicated in the International Standards appropriate to the spices and condiments concerned. 1 Scope and field of application This International Standard specifies a method for the quantitative determination of
16、 filth in spices and condiments. As no limits have been prescribed for filth in International Standards on spices and condiments, this method should be used for collecting more data and for settling international disputes. 2 Reference ISO 948, Spices and condiments Sampling. 3 Definition For the pur
17、pose of this International Standard, the following definition applies. filth mineral matter (sand, soil) and matter of animal origin (insect fragments, rodent hairs and excreta) separated from the product under the conditions specified 4 Principle Washing the product with chloroform (after, if neces
18、sary, preliminary extraction with light petroleum) and examination of the washings for heavy filth and sand. Washing the product with water, with or without treatment with pancreatin enzyme, and agitation with light petroleum, the light filth collecting at the interface between the liquids after sep
19、aration. Transference of the light filth to a filter paper and microscopical examination for contaminants such as insect fragments and rodent hairs. 5 Reagents The water used shall be distilled water or water of at least equivalent purity. 5.1 Chloroform and, if required (see 8.3), chloroform/carbon
20、 tetrachloride mixtures. 5.2 Pancreatin solution Use pancreatin complying with the requirements of the Annex, and which has been kept at about10 C. Use a solution which has been freshly prepared as follows. Mix10g of pancreatin with100ml of warm water (temperature not exceeding40 C). Stir mechanical
21、ly for10min or allow to stand for30min with intermittent stirring. Pour the solution through a loosely packed pad of cotton wool, 100mm thick, in a60 funnel of diameter100to125mm. Repeat the filtration through the same pad. If filtration is slow in either case, filter with suction through a fast fil
22、ter paper using a Buchner funnel. If the filtration is still slow, pour the solution through a slightly compressed cotton wool plug in the 60 funnel. Repeat if necessary, until the solution filters rapidly through paper. (Soluble pancreatin may be filtered directly through paper with suction.) Dilut
23、e the flitrate to100ml for each10g portion. 5.3 Trisodium orthophosphate, 50g/l solution. 5.4 Formaldehyde solution 5.5 Light petroleum, boiling range40to60 C. 5.6 Light petroleum, boiling range100to120 C. 6 Apparatus Usual laboratory apparatus, and 6.1 Trap flask (Wildman), consisting of a1000ml co
24、nical flask into which is inserted a close-fitting rubber stopper carried on a rigid metal rod,5mm in diameter and approximately100mm longer than the height of the flask. (A rod of a greater diameter is not desirable because of its greater displacement of liquid.) The rod is threaded at its lower en
25、d and furnished with nuts and washers to hold it in place on the stopper. The lower nut and washer are countersunk in the rubber to prevent them from striking the flask. See the figure. Alternatively, a separating funnel, of capacity1000ml, may be used. 6.2 Beakers, of capacity600ml. 6.3 Buchner fun
26、nel, of diameter15cm with a filter paper. 6.4 Buchner funnel, of diameter7cm with a filter paper ruled with parallel lines5mm apart. 6.5 Filter paper, ashless.BS4585-14:1983 2 BSI 10-1999 6.6 Crucible, tared. 6.7 Oven, capable of being controlled at80 C. 6.8 Oven, capable of being controlled at103 C
27、. 6.9 Petri-dish, of diameter80mm. 6.10 Suitable magnifying device (microscope, binocular magnifier, etc. or preferably a wide-field stereoscopic microscope). 6.11 Balance 7 Sampling Sample the material by the method specified in ISO 948. 8 Procedure NOTETo achieve a satisfactory separation of the l
28、ight filth from spice tissue, it may be necessary to remove most of the volatile oil and fat, or to treat the test portion with pancreatin enzyme to digest starch and protein, or both. If removal of volatile oil or fat is required, proceed as described in8.2; otherwise, proceed directly as described
29、 in 8.3. 8.1 Test portion Ensure that the test portion is representative of the laboratory sample (final lot sample). 8.1.1 Whole and broken spices Break the material into small pieces, weigh, to the nearest0,1g,25g of the sample and transfer it to a breaker (6.2). 8.1.2 Ground spices Weigh, to the
30、nearest0,1g,25g of the sample and transfer it to a beaker (6.2). 8.2 Preliminary removal of volatile oil and fat Add200ml of the light petroleum (5.5) to the test portion (8.1) in the beaker. Boil gently on a warm water bath for15min. Remove the light petroleum by decanting, taking care not to lose
31、any of the material under test. 8.3 Separation of heavy filth and sand Add400ml of the chloroform (5.1) to the test portion (8.1) or to the residue from the operation described in 8.2. Allow the beaker to stand for at least1h with occasional stirring. Transfer the material and the solvent to the Buc
32、hner funnel(6.3), leaving the heavy residue of sand and soil in the beaker. Drain. If appreciable spice tissue remains on the bottom of the beaker, add successive portions of chloroform mixed with carbon tetrachloride to give increasingly higher relative densities until practically all spice tissue
33、has been removed by flotation. Transfer the heavy residue from the beaker to the ashless filter paper (6.5) and wash it with water to remove any sodium chloride present in the spice. Examine this residue. If there is an appreciable residue, place the filter paper in the tared crucible (6.6), ignite,
34、 and weigh the sand and soil. 8.4 Treatment of residue retained on the Buchner funnel Dry the material retained on the Buchner funnel (see 8.3) for 1 h in the oven (6.7), controlled at80 C. 8.4.1 Procedure without enzyme treatment Transfer the residue to the trap flask (6.1). Add about150ml of water
35、, heat to boiling and simmer for15min with stirring. Wash down the inside of the flask with water and cool to below20 C, diluting to about600ml with water. 8.4.2 Procedure with enzyme treatment Transfer the dry residue to a beaker (6.2). Add300ml of water and stir until homogeneous. Add50ml of the p
36、ancreatin solution (5.2) and mix. Adjust to pH8with the trisodium orthophosphate solution (5.3). Readjust the pH after about15min, and again after about45min. Add5drops of the formaldehyde solution (5.4) and allow to digest overnight at37to40 C. Cool and transfer to the trap flask (6.1), making up t
37、o about 600 ml with water. 8.5 Separation of light filth 8.5.1 Add, down the stirring rod of the flask,25ml of the light petroleum (5.6). Tilt the trap flask at about45 to the vertical and mix for1min at the rate of4strokes per second with a brisk rotary motion so that the liquid is brought to a rol
38、l. Avoid splashing through the surface of the liquid in the trap flask with the rubber stopper. Allow to stand for5min. Then fill the flask with water and allow to stand for30min. Stir every5min.BS4585-14:1983 BSI 10-1999 3 8.5.2 Spin the stopper to remove sediment and raise the stopper as far as po
39、ssible into the neck of the flask, making sure that the light petroleum layer and at least1cm of the liquid below the interface are above the stopper. Holding the stopper in place, transfer the trapped liquid to the Buchner funnel(6.4). Filter. 8.5.3 Add15ml of the light petroleum (5.6) to the conte
40、nts of the trap flask and mix thoroughly. After15min, repeat the operations described in8.5.2. If this second extraction yields an appreciable quantity of filth, decant most of the liquid from the flask, add another15ml of the light petroleum (5.6) and carry out a third extraction. 8.6 Microscopical
41、 examination of light filth Remove the filter paper from the Buchner funnel and place it on the petri-dish (6.9). Place the petri-dish in the oven (6.8), controlled at103 C, for30min. The dried filter paper should be tightly stuck to the petri-dish. Examine the entire area of the filter paper, using
42、 the magnifying device (6.10) in reflected light, scraping and probing with a mounted needle. Carry out the examination from left to right, from top to bottom for the first interval, from bottom to top for the second interval, from top to bottom for the third interval, etc. 9 Expression of results 9
43、.1 Heavy filth (see 8.4) Note the presence of mineral matter. If the amount of sand and soil is such as to require calcination and weighing of these impurities, the mineral impurities content of the product, expressed as a percentage by mass, is equal to where 9.2 Light filth (see 8.6) Note the pres
44、ence of matter of animal origin (see8.6). If required, record separately the numbers of insect fragments, rodent hairs and other items of animal origin in the test portion, i.e. the numbers per25g of sample. 10 Test report The test report shall show the method used and the results obtained. It shall
45、 also mention any operating conditions not specified in this International Standard, or regarded as optional, as well as any circumstances that may have influenced the results. The test report shall include all the information necessary for the complete identification of the sample. m 1 100 m 0 - m
46、0 is the mass, in grams, of the test portion; m 1 is the mass, in grams, of the residue obtained (8.3).BS4585-14:1983 4 BSI 10-1999 NOTEThe upper nut and washer have been omitted. Figure Wildman trap flask (6.1), showing method of useBS4585-14:1983 BSI 10-1999 5 Annex Pancreatin Specification A.0 Ge
47、neral Pancreatin is a substance containing enzymes, principally pancreatic amylase, trypsin, and pancreatic lipase, obtained from the pancreas of the hog, Sus scrofa Linne var. domesticus Gray (Fam. Suidae), or of the ox, Bos taurus Linne (Fam. Bovidae). Pancreatin converts not less than25times its
48、mass of N.F. 1)Potato Starch Reference Standard into soluble carbohydrates, and not less than25times its mass of casein into proteoses. Pancreatin of a higher digestive power may be brought to this standard by admixture with lactose, or with sucrose containing not more than3,25% of starch, or with p
49、ancreatin of lower digestive power. A.1 Description Pancreatin occurs as a cream-coloured, amorphous powder, having a faint, characteristic, but not offensive odour. Pancreatin changes protein into proteoses and derived substances, and converts starch into dextrins and sugars. Its greatest activities are in neutral or faintly alkaline media; more than traces of mineral acids or large amounts of alkali hydroxides render it inert. An excess of alkali carbonate inhibits its action. A.2 Assay for fat Introduce2gof pancreatin into a flask o
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