EN ISO 12872-2014 en Olive oils and olive-pomace oils - Determination of the 2-glyceryl monopalmitate content《橄榄油和橄榄果渣油 2-甘油单棕榈酸酯的测定(ISO 12872 2010)》.pdf

1、BS ISO12872:2010ICS 67.200.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDOlive oils andolive-pomace oils Determinationof the 2-glycerylmonopalmitate contentBS EN ISO 12872:2014BS EN ISO 12872:2014ISBN 978 0 580 83969 6Amendments/corrigenda issued since publi

2、cationDate Comments30 April 2014 This corrigendum renumbers BS ISO 12872:2010 as BS EN ISO 12872:2014This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 June 2010 The British Standards Institution 2014. Published by BSI Standards Limited 2014N

3、ational forewordThis British Standard is the UK implementation of EN ISO 12872:2014. It is identical to ISO 12872:2010. It supersedes BS ISO 12872:2010, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee AW/307, Oilseeds, animal and vegetable fats and oil

4、s and their by-products.A list of organizations represented on this committee can be obtained on request to its secretary.The publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard canno

5、t confer immunity from legal obligations.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 12872 April 2014 ICS 67.200.10 English Version Olive oils and olive-pomace oils - Determination of the 2-glyceryl monopalmitate content (ISO 12872:2010) Huiles dolive et huiles de grignons dolive - Dter

6、mination de la teneur en 2-glycryl monopalmitate (ISO 12872:2010)Olivenle und Oliventresterle - Verfahren zur Bestimmung des Prozentanteiles von 2-Glyceryl Monopalmitat in Olivenlen (ISO 12872:2010) This European Standard was approved by CEN on 11 April 2014. CEN members are bound to comply with the

7、 CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management

8、 Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status a

9、s the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Ne

10、therlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All

11、rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 12872:2014 EBS ISO 12872:2010ISO 12872:2010(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed

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14、use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2010 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized i

15、n any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 2

16、2 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2010 All rights reservedEN ISO 12872:2014 (E) 3 Foreword The text of ISO 12872:2010 has been prepared by Technical Committee ISO/TC 34 “Food products” of the International Organization for Standardization (ISO) and h

17、as been taken over as EN ISO 12872:2014 by Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products - Methods of sampling and analysis” the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either

18、 by publication of an identical text or by endorsement, at the latest by October 2014, and conflicting national standards shall be withdrawn at the latest by October 2014. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or

19、 CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech R

20、epublic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. E

21、ndorsement notice The text of ISO 12872:2010 has been approved by CEN as EN ISO 12872:2014 without any modification. BS EN ISO 12872:2014EN ISO 12872:2014 (E)BS ISO 12872:2010ISO 12872:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3

22、 Terms and definitions .1 4 Principle1 5 Reagents.1 6 Apparatus.2 7 Sampling.3 8 Preparation of the test sample.3 9 Procedure.4 9.1 Preparatory steps 4 9.2 Column chromatography4 9.3 Hydrolysis with pancreatic lipase4 9.4 Preparation of the silylated derivatives and gas chromatography 5 9.5 Gas chro

23、matography 5 10 Expression of results5 11 Precision.6 11.1 Interlaboratory test6 11.2 Repeatability 6 11.3 Reproducibility 6 12 Test report6 Annex A (informative) Chromatograms 7 Annex B (informative) Results of an interlaboratory test .10 Annex C (informative) Preparation and activity of the lipase

24、.11 Bibliography13 BS ISO 12872:2010ISO 12872:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword ivIntroduction.v1 Scope2 Normative references.3 Terms and definitions .4 Principle5 Reagents.16 Apparatus.27 Sampling.8 Preparation of the test sample.39 Procedure.4 9.1 Preparatory steps 4 9

25、.2 Column chromatography4 9.3 Hydrolysis with pancreatic lipase4 9.4 Preparation of the silylated derivatives and gas chromatography 5 9.5 Gas chromatography 10 Expression of results511 Precision.6 11.1 Interlaboratory test6 11.2 Repeatability 6 11.3 Reproducibility 12 Test report6A Chromatograms 7B

26、 Results of an interlaboratory test .10Annex C (informative) Preparation and activity of the lipase.11Bibliography13 BS EN ISO 12872:2014ISO 12872:2010(E)BS ISO 12872:2010ISO 12872:2010(E) iv ISO 2010 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide

27、 federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that

28、committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in acc

29、ordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requ

30、ires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 12872 was prepared by Technic

31、al Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils. BS ISO 12872:2010ISO 12872:2010(E) ISO 2010 All rights reserved vIntroduction As part of the Trade standard applying to olive oils and olive-pomace oils, the International Olive Council OC) published COI/T

32、.20/Doc. 23:20066. COI/T.20/Doc. 23 was applicable to olive and olive-pomace oils and was used to distinguish between lampante virgin olive oils and crude olive-pomace oils. Olive pomace is the residual paste which still contains a variable amount of water and oil after pressing or centrifuging. In

33、2008, the IOC submitted the document to ISO/TC 34/SC 11 for adoption as an International Standard. BS EN ISO 12872:2014ISO 12872:2010(E)BS ISO 12872:2010INTERNATIONAL STANDARD ISO 12872:2010(E) ISO 2010 All rights reserved 1Olive oils and olive-pomace oils Determination of the 2-glyceryl monopalmita

34、te content 1 Scope This International Standard specifies a procedure for the determination of the content, as a percentage mass fraction, of 2-glyceryl monopalmitate in olive oils and olive-pomace oils that are liquid at ambient temperature (20 C). NOTE This International Standard is based on COI/T.

35、20/Doc. 23:20066. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 661,

36、 Animal and vegetable fats and oils Preparation of test sample 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 2-glyceryl monopalmitate content mass fraction of 2-glyceryl monopalmitate in the monoacylglycerol fraction, determined according t

37、o the method specified in this International Standard NOTE The 2-glyceryl monopalmitate content is expressed as a percentage. 4 Principle The oil, after suitable preparation, is subjected to the action of pancreatic lipase. A partial hydrolysis takes place that is specific for positions 1 and 3 of t

38、he triacylglycerol molecule so that 2-monoacylglycerols are obtained as reaction products. The percentage of 2-glyceryl monopalmitate in the monoacylglycerol fraction is determined, after silylation, by capillary gas chromatography. 5 Reagents WARNING Comply with any local regulations which specify

39、the handling of hazardous substances. Technical, organizational and personal safety measures shall be followed. During the analysis, unless otherwise stated, use only reagents of recognized analytical grade, and distilled or demineralized water or water of equivalent purity. BS EN ISO 12872:2014ISO

40、12872:2010(E)BS ISO 12872:2010ISO 12872:2010(E) 2 ISO 2010 All rights reserved5.1 Silica gel, with a particle size of 0,063 mm to 0,200 mm (70/280 mesh), prepared as follows: put the silica gel into a porcelain cup, dry in an oven at 160 C for 4 h, then cool at ambient temperature in a desiccator. A

41、dd a volume of water equivalent to 5 % of the mass of the silica gel as follows: weigh 152 g of silica gel into a 500 ml Erlenmeyer flask, add 8 g of water, stopper and homogenize carefully. Leave to settle for at least 12 h before using. 5.2 n-Hexane, chromatography grade. 5.3 Isopropanol. 5.4 Isop

42、ropanol-water mixture, volume fractions 50 ml/100 ml. 5.5 Pancreatic lipase, activity between 2,0 and 10 lipase units per milligram (see Annex C). 5.6 Buffer solution of tris(hydroxymethyl)aminomethane: prepare an aqueous solution (1 mol/l) with pH 8 and mix with concentrated HCl, volume fractions 5

43、0 ml/100 ml. 5.7 Sodium cholate, special enzyme grade, aqueous solution, mass fraction 0,1 g/100 g. Use this solution within 15 days of preparation. 5.8 Calcium chloride, aqueous solution, mass fraction 22 g/100 g. 5.9 Diethyl ether, chromatography grade. 5.10 Elution solvent: mixture of n-hexane-di

44、ethyl ether, volume fraction of n-hexane 87 ml/100 ml and of diethyl ether 13 ml/100 ml. 5.11 Sodium hydroxide, aqueous solution, mass fraction 12 g/100 g. 5.12 Phenolphthalein, ethanolic solution, mass concentration 1 g/100 ml. 5.13 Carrier gas: hydrogen or helium, gas chromatography grade. 5.14 Au

45、xiliary gases: hydrogen, free from moisture and organic substances, and synthetic air, gas chromatography grade. 5.15 Silylation reagent: mixture of pyridine, hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS); volume fractions: 9 ml/13 ml, 3 ml/13 ml, and 1 ml/13 ml, respectively. 5.16 Re

46、ference samples: pure monoacylglycerols and mixtures of monoacylglycerols with a known composition similar to that of the sample. 6 Apparatus Usual laboratory equipment and in particular the following. 6.1 Erlenmeyer flasks, of capacity 25 ml. 6.2 Beakers, of capacities 100 ml, 250 ml, and 300 ml. 6

47、.3 Glass chromatography column, 21 mm to 23 mm internal diameter, 400 mm in length, with septum and stopcock. 6.4 Measuring cylinders, of capacities 10 ml, 50 ml, 100 ml, and 200 ml, ISO 47882class A. 6.5 Round-bottomed flasks, of capacities 100 ml and 250 ml. 6.6 Rotary evaporator. BS EN ISO 12872:

48、2014ISO 12872:2010(E)BS ISO 12872:2010ISO 12872:2010(E) ISO 2010 All rights reserved 36.7 Centrifuge tubes, conical bottom, of capacity 10 ml, with ground-glass stopper. 6.8 Centrifuge, suitable for 10 ml and 100 ml tubes. 6.9 Water bath, capable of maintaining a temperature of (40 0,5) C. 6.10 Grad

49、uated pipettes, of capacities 1 ml and 2 ml, ISO 8351class A. 6.11 Hypodermic syringe, 1 ml. 6.12 Microsyringe, 100 l. 6.13 Separating funnel, 1 000 ml. 6.14 Gas chromatograph, suitable for use with capillary columns, equipped with the components specified in 6.14.1 to 6.14.5. 6.14.1 Cold on-column injector. 6.14.2 Flame ionization detector. 6.14.3 Column oven, capable of maintaining the temperature to within 1 C. 6.14.4 Computer-based integration system. 6.14.5 Fused silica capillary column, of length 8 m to 12