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1、BRITISH STANDARD BS ISO 17059:2007 Oilseeds Extraction of oil and preparation of methyl esters of triglyceride fatty acids for analysis by gas chromatography (Rapid method) ICS 67.200.20 ? Licensed Copy: London South Bank University, London South Bank University, Sat Aug 18 09:50:18 GMT+00:00 2007,
2、Uncontrolled Copy, (c) BSI BS ISO 17059:2007 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2007 BSI 2007 ISBN 978 0 580 55087 4 National foreword This British Standard is the UK implementation of ISO 17059:2007. The UK participati
3、on in its preparation was entrusted to Technical Committee AW/307, Oil seeds, animal and vegetable fats and oils and their by products. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary pr
4、ovisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Amendments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Sat Aug 18
5、 09:50:18 GMT+00:00 2007, Uncontrolled Copy, (c) BSI Reference number ISO 17059:2007(E) INTERNATIONAL STANDARD ISO 17059 First edition 2007-07-01 Oilseeds Extraction of oil and preparation of methyl esters of triglyceride fatty acids for analysis by gas chromatography (Rapid method) Graines olagineu
6、ses Extraction de lhuile et prparation des esters mthyliques dacides gras de triglycrides pour analyse par chromatographie en phase gazeuse (Mthode rapide) BS ISO 17059:2007 Licensed Copy: London South Bank University, London South Bank University, Sat Aug 18 09:50:18 GMT+00:00 2007, Uncontrolled Co
7、py, (c) BSI ii Licensed Copy: London South Bank University, London South Bank University, Sat Aug 18 09:50:18 GMT+00:00 2007, Uncontrolled Copy, (c) BSI iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). T
8、he 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 committee. International organizations, governmental and non-go
9、vernmental, 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 accordance with the rules given in the ISO/IEC Directives, Part 2.
10、 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 requires approval by at least 75 % of the member bodies casting a v
11、ote. 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 17059 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 2, Oleag
12、inous seeds and fruits and oilseed meals. BS ISO 17059:2007 Licensed Copy: London South Bank University, London South Bank University, Sat Aug 18 09:50:18 GMT+00:00 2007, Uncontrolled Copy, (c) BSI iv Introduction Chromatographic analysis of the fatty acid methyl esters (FAME) of oilseeds requires o
13、il extraction from the oilseeds. To date, no International Standard has specified a method for extracting oil from oilseeds for FAME analysis. The methods usually performed in laboratories involve oil extraction for the determination of oil content and are tedious or time consuming2, 3. Consequently
14、, the total duration and cost of the analysis of triglyceride fatty acids in oilseeds, including oil extraction, preparation and gas chromatography of the FAME are considerably increased by the oil extraction step. This International Standard specifies a rapid and optimized method for a combined oil
15、 extraction and FAME preparation. The oil is only partially extracted from the seeds and the extracted fraction remains representative enough of the total content when the method is applied to the seeds specified in the Scope4, 5. The FAME are prepared according to the transesterification method des
16、cribed in ISO 5509 and slightly modified to be applied to iso-octane solutions of oil. Taking into account that no reference method for oil extraction exists, the oil extraction method specified in this International Standard was compared to ISO 6592 in an interlaboratory test6. Results showed very
17、good agreement between the two methods except when applied to rapeseed with high erucic acid content. In this case, this method led to values of erucic acid content higher by approximately a mass fraction of 1 %. BS ISO 17059:2007 Licensed Copy: London South Bank University, London South Bank Univer
18、sity, Sat Aug 18 09:50:18 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 1 Oilseeds Extraction of oil and preparation of methyl esters of triglyceride fatty acids for analysis by gas chromatography (Rapid method) 1 Scope This International Standard specifies a rapid method for extraction of oil and for
19、preparation of the methyl esters of fatty acids. The methyl esters thus obtained can be used for gas chromatography. This International Standard is applicable to the following oilseeds: rape, sunflower, soya beans, mustard, linseed. NOTE Applying this rapid method to high erucic acid content rapesee
20、d leads to an overestimation of erucic acid content by approximately a mass fraction of 1 %. 2 Normative references The following referenced documents are indispensable for the application of this International Standard. For dated references, only the edition cited applies. For undated references, t
21、he latest edition of the referenced document (including any amendments) applies. ISO 664, Oilseeds Reduction of laboratory sample to test sample ISO 5509:2000, Animal and vegetable fats and oils Preparation of methyl esters of fatty acids 3 Principle The oil is cold extracted from previously crushed
22、 grains by shaking in iso-octane. After filtration, the triglyceride fatty acids present in the iso-octane solution are transesterified with potassium hydroxide into methyl esters. 4 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. 4.1 Iso-octane (2,2,4-trimethy
23、lpentane) of chromatographic quality. See Annex A. 4.2 Anhydrous sodium sulfate. 4.3 Other reagents used for the preparation of the methyl esters are specified in ISO 5509:2000, 5.3.1 and 5.3.3. BS ISO 17059:2007 Licensed Copy: London South Bank University, London South Bank University, Sat Aug 18 0
24、9:50:18 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 2 5 Apparatus Usual laboratory apparatus and, in particular, the following. 5.1 Blade crusher, coffee grinder type. 5.2 Test tubes, of glass, of capacity 10 ml, with ground or screw type stopper and PTFE cap. 5.3 Graduated pipette, of capacity 5 ml.
25、 5.4 Pasteur pipettes, of length 150 mm, filled with a glass wool wick and anhydrous sodium sulfate up to a height of 20 mm. 5.5 Test tubes, of glass, of capacity 5 ml, with ground or screw type stopper and PTFE cap. 5.6 Glass vial, of capacity 2 ml, with screw type stopper and PTFE cap. 6 Sampling
26、A representative sample should have been sent to the laboratory. It should not have been damaged or changed during transport or storage. Sampling is not part of the method specified in this International Standard. A recommended sampling method is given in ISO 5421. 7 Procedure 7.1 Preparation of the
27、 test sample Reduce the sample in accordance with ISO 664 and crush a quantity of approximately 10 g using a blade crusher (5.1) during 15 s. NOTE For samples that are non-homogeneous in nature, i.e. contain significant quantities of unseparable seeds (such as Sinapis arvensis in canola) a larger sa
28、mple (25 g) may be required to ensure an accurate estimate of fatty acids. 7.2 Test portion 7.2.1 General The crushed material test portion shall be adapted as a function of the oil content of the sample in order to permit the extraction of approximately 100 mg of oil. 7.2.2 Case of grains having an
29、 oil content exceeding 30 % by mass (rape, mustard, sunflower and linseed) Mix the crushed material and weigh, to the nearest 0,02 g, approximately 0,40 g of it in a 10 ml test tube (5.2). 7.2.3 Case of grains having an oil content between 15 % and 30 % by mass (soya beans) Mix the crushed material
30、and weigh, to the nearest 0,04 g, approximately 0,80 g of it in a 10 ml test tube (5.2). BS ISO 17059:2007 Licensed Copy: London South Bank University, London South Bank University, Sat Aug 18 09:50:18 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 3 7.3 Extraction of the oil Using a pipette (5.3), add
31、5 ml of iso-octane (4.1) to the tube containing the crushed material and stopper. Shake for 2 min, leave to settle or centrifuge if necessary. If the supernatant of the extract is not clear, proceed with filtration and drying (7.4). If the supernatant of the extract is clear, filtration and drying a
32、re not necessary and may be omitted. Transfer 3 ml of the supernatant to a 5 ml test tube (5.5). The extract is then ready for the preparation of the methyl esters (7.5). 7.4 Filtration and drying of the extract Place the Pasteur pipette (5.4) containing anhydrous sodium sulfate (4.2) above a 5 ml t
33、est tube (5.5). Transfer the supernatant of the extract (7.3) to the Pasteur pipette and allow to drain off to obtain a volume of approximately 3 ml of clear extract in the test tube. This extract is then ready for the preparation of the methyl esters (7.5). 7.5 Preparation of the methyl esters Proc
34、eed according to ISO 5509:2000, from 5.6.2.2 to 5.6.2.4 on the extract prepared in the 5 ml test tube (7.3 or 7.4). NOTE The reagents are specified in ISO 5509:2000, 5.3.1 and 5.3.3. Transfer (with dilution or not, according to ISO 5509:2000, 5.6.2.4 and the injection mode in gas chromatography) the
35、 supernatant containing the methyl esters into a 2 ml glass vial (5.6) with stopper. The solution is ready to inject into the gas chromatograph. 8 Test report The test report shall specify: all information necessary for the complete identification of the sample; the sampling method used, if known; t
36、he test method used, with reference to this International Standard; all operating details not specified in this International Standard, or regarded as optional, together with details of any incidents which may have influenced the test result(s). BS ISO 17059:2007 Licensed Copy: London South Bank Uni
37、versity, London South Bank University, Sat Aug 18 09:50:18 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 4 Annex A (normative) General analytical procedures A.1 Reagents The reagents shall not produce peaks that interfere with those of the methyl esters of fatty acids during gas- liquid chromatography.
38、 Consequently, any new batch of reagent or solvent should be checked by using it to prepare the methyl esters of pure oleic acid and analysing them by gas-liquid chromatography. If any extra peaks appear, the reagent should be rejected. A.2 Storage of methyl ester solution The esters should preferab
39、ly be analysed as soon as possible. If necessary, the iso-octane solution containing the methyl esters may be stored under inert gas in a refrigerator. For a longer period of storage, it is advisable to protect the methyl esters against autoxidation by adding to the solution an antioxidant in such a
40、 concentration as will not interfere with the subsequent analysis, for example a 0,05 g/l solution of BHT (2,6-di-t-butyl-4-methylphenol). BS ISO 17059:2007 Licensed Copy: London South Bank University, London South Bank University, Sat Aug 18 09:50:18 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 5 Bib
41、liography 1 ISO 542:1990, Oilseeds Sampling 2 ISO 659:1998, Oilseeds Determination of oil content (Reference method) 3 XP V 03-030:1991 (French standard), Agricultural products and foodstuffs Extraction of the crude fat with a view to its characterization 4 BLIN, F, 1998. Rapid extraction of oil fro
42、m oilseeds with a view to the analysis of fatty acids. Report- CETIOM 5 QUINSAC, A. and BLIN, F. Validation of a rapid method to extract oil in oleaginous seeds for fatty acid analysis. Proceedings of the 10th International Rapeseed Congress, Camberra, Australia, September 26 to 29, 1999, 122 6 CETI
43、OM, 2002, Report of the Ring-Test (January - April 2001): Comparison between ISO/WD 17059 and ISO 659 ISO 5509 7 ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions 8 ISO 5725-2:1994, Accuracy (trueness and precision) of me
44、asurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method BS ISO 17059:2007 Licensed Copy: London South Bank University, London South Bank University, Sat Aug 18 09:50:18 GMT+00:00 2007, Uncontrolled Copy, (c) BSI B
45、S ISO 17059:2007 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions
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