EN 1528-2-1996 Fatty Food - Determination of Pesticides and Polychlorinated Biphenyls (PCBs) - Part 2 Extraction of Fat Pesticides and PCBs and Determination of.pdf

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1、 STD-BSI BS EN 1528-2-ENGL 2797 II Lb2YbbS Ob222Y7 772 U BRITISH STANDARD Fatty food - Determination of pesticides and polychlorinated biphenyls (PCBs) Part 2. Extraction of fat, pesticides and PCBs, and determination of fat content The European Standard EN 15282 : 1996 has the status of a British S

2、tandard ICs 67.040 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGIW LAW BS EN 1528-2 : 1997 STD*BSI BS EN 1528-2-ENGL 1777 M lb24bb7 Ob22250 973 AmdNo. BS EN 1628-2 : 1997 Date Text affected Committees responsible for this British Standard The preparation of this British standard w

3、as entrusted to Technical Panel AWM, Food analysis - Horizontal methods, upon which the foliowing bodies were represented Association of public Adysfs Department of We and Industqy (Laboratory of the Government Chemist) Food and Drink Federation Instut of Food Science and Technology Minishy of Agric

4、uiture Fisheries and Food Royal Society of Chemistxy This British Standard, having been prepared under the direction of the Consumer Products and SeMces Sector Board, was pubiished under the authority of the Standards Board and comes into effect on 15 June 1997 Q BSI 1997 The foiiowing BSI reference

5、s relate to the work on this Stan* Committee reference Awl43 Draft for comment 94h06376 DC ISBN O 580 27380 6 STD*BSI BS EN 1528-2-ENGL 1947 lb24bb9 Ob22251 32T BS EN 1528-2 : 1997 Contents page Committees responsible Inside front cover National foreword ii Foreword 2 Text of EN 15282 3 lk lk m O BS

6、I 1997 1 STD-BSI BS EN L528-2-ENGL 1177 1111 Lb24bb9 Ob22252 2bb = BS EN 1528-2 : 1997 National foreword This British Standard has been prepared by Technical Committee AW/B and is the English language version of EN 15282 : 1996 Fatty food - Determination of pesticides and polychlorinated biphenyls (

7、PCBs) Part 2 : Extmctwn of fat, pesticides and PCBs, and deterrninath of fat content published by the European Committee for Standardhiion (CEN). EN 15282 was produced as a result of inteniational discussions in which the United Kingdom took an active part Cross-references Publication referred to EN

8、 15281 : 1996 EN 1528-3 : 1996 EN 15284 : 1996 Corresponding British Standard BS EN 15281 : 1997 Fatty food - Determinath of pesticides and polychlorinated biphenyls (PCBs) Part 1 : General BS EN 15283 : 1997 Fattyfood - Determinath of pesticides and polychlorinated biphenyls (PCBs) Part 3 : Clean-u

9、p methods BS EN 15284 : 1997 Fatty food - Determinath of pesticides and polychlorinated biphenyls (PCBs) Part 4 : Determination, confimtorg tests, miscellaneous Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a fr

10、ont cover, an inside front cover, pages i and ii, the EN title page, pages 2 to 8, an inside back cover and a back cover. u O BSI 1997 bt bt v1 STD-BSS BS EN 1528-2-ENGL 1777 9 1b24bb9 Ob22253 IT2 EUROPEAN STANDARID EN 1528.2 NOEWIE EUROPENNE EUROP NORM November 1996 ICs 67.040 Descriptors: Food pro

11、ducts, edible fats, chemical analysis, determination of content, pesticides, polychlorobiphenyl, fats, extraction English version Fatty food - Determination of -cides and polychlorinated biphenyls (PCE3s) - Part 2 : Extmction of fbt, pesticides and PCBs, and determination of fat content Aliments gra

12、s - Dosage des paticides et des polychlombiphnyles (PCB) - Me 2 : Exhadion de la c) reflux condenser; d) heat source (for example a heating mantle). 6.14 Sand or water bath, capable of being controlled between ambient temperature and 100 “C. 6.16 Bmshte bottles, 250 ml, glass. 6.16 Extmtion tube, co

13、mprisiig a glass tube of internai diameter 12 mm and of length 300 mm, having a capiilary exit below, and at the upper end a section of length 100 mm of internai diameter 50 mm. 6.17 Extraccion hirnbles (optionai). The use of extsaction thimbles can often resuit in the presence of impurities in the

14、sample extracts (iterference peaks in the gas chmatogram). They should therefore be preextracted with solvent of the highest purity and stored in an aii-giass container. 6.18 Sepamting funnels, of capacity 500 ml and 1000 ml. 6.19 Sintered glass funnels, of capacity 80 ml, disk diameter 4 cm. 6.20 V

15、olumetricjashs, of suitable capacity, e.g. 5 ml, 10 ml. 6.21 Cotton wool and glass wool, chemically pure. Before use, extract with n-hexandacetone and store in a well-stoppered flask. 6.22 Fterpapw, round, of diameter approximately 30 cm, sufficiently solvent washed. 6.23 Mortar and pesuisfer 30 g o

16、f the sample into a 500 ml beaker and add enough sodium sulfate (4.14) to give a friable mixture. Add 300 ml of a 2 : 1 (Vm mixhire of n-hexane (4.8) and acetone (4.1), tmnsfer to a blender cup and blend the mixture for 3 min. Decant the exbract through a funnel containing a plug of cotton wool into

17、 a 1000 ml separating funnel (5.18). Re-blend the sample residue with a further 150 ml portion of the 2 : 1 nihexane-acetone mjxture and decant through the cotton wool plug into the separating funnel. Add 250 ml of sodium sulfate solution (4.11) and shake the funnel for 30 s. Allow the iayers to sep

18、arate and discard the lower, aqueous layer. Wash the upper layer in the separating funnel with another 250 ml portion of sodium sulfate solution. Pass the n-hexane layer through a sintered glass funnel (6.19) containing approximately 20 g of sodium suifate into a round-bottomed flask, and evaporate

19、the solution in a rotary evaporator at about 50 “C under reduced pressure. Remove sohrent residues by using a gentle stxeam of nitrogen. 6.4.6 Partitioning extraction forjkh and crabs 4 Macerate the crab pancreatic tissue or sh entrails sample in a blender to mix the sample thoroughiy Weigh out appr

20、oximately 25 g of crab or 100 g of fish tissue. Add 200 g of sodium suJfate (4.14) and mix with a sthing rod until a friable mixture is obtained. To the samplemass,add200mlofa3:1(VN)mixtureof niheme (4.8) and acetone (4.1) and heat on the water bath under reflux for 20 min with constant stimng. Pour

21、 the solvent into a separating funnel containing 500 ml of the sodium sulfate solution (4.11). Carry out the extraclion two more times, each with a 150 ml portion of the 3 : 1 niheme-acetone mixture. Combine ail the extracts in the separating funnel. Shake the funnel for 30 s, and allow the two phas

22、es to separate. Drain the lower aqueous layer and discard it. Add a further 500 ml of the sodium sulfate solution and repeat the washing procedure. Run the remaining organic layer through a sintered glass funnel (5.19) containing approximately 15 g of sodium sulfate into a round-bottomed flask and e

23、vaporate the solution in a rotary evaporator at about 50 “C under reduced pressure. Remove solvent residues by using a gentle stream of nitrogen. O BSI 1997 STD-BSI BS EN L52a-Z-ENGL 1997 Lb2YbbS 3b22259 110 Page 7 EN 15282 : 1996 6.4.6 Cold centrtficgation extraction 5 glycine bufer solution (4.10)

24、 and 50 1 of enzyme suspension (4.9). incubate at (37 agitating gently li-ansfer the sample to a 600 mi beaker, 6.4.6.1 Meat und fish To 20 g of meat or fish, add 10 g of sodium sulfate add 250 mi of a 3 : 1 (VIV) mixture of n-hexane and (4.14) and 50 mi of n-hexane (4-8). Homogenize ad acetone, and

25、 homogenize for 2 min. MOW the phases centrifuge for 6 min at 1500 min-l. Decant the to separate and decant the solvent mixture through a supernatant solution and repeat the exIraction funnel containing a small plug of cotton wool into with 50 ml of n-hexane. Combine both extracts, rotary a 500 ml s

26、epmg funnel containing 250 mi of sodium evaporate the n-hexane layer at 35 “C to sulfate solution (4.11). Add a further 50 ml of the 3 : 1 prximate 1 ml and remove solvent residues mhem+a Fax: 0181 996 7400. BSI offers members an individual updating service called PLUS which ensures that subscribers

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