1、AReference numberISO 11025:1998(E)INTERNATIONALSTANDARDISO11025First edition1998-02-01Oil of cassia, Chinese type Determinationof trans-cinnamaldehyde content Gaschromatographic method on capillarycolumnsHuile essentielle de cannelle type Chine Dtermination de la teneur entrans-cinnamaldhyde Mthode
2、par chromatographie en phase gazeusesur colonne capillaireCopyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-ISO 11025:1998(E) ISO 1998All rights reserved. Unless otherwise
3、specified, no part of this publication may be reproducedor utilized in any form or by any means, electronic or mechanical, including photocopying andmicrofilm, without permission in writing from the publisher.International Organization for StandardizationCase postale 56 CH-1211 Genve 20 SwitzerlandI
4、nternet centraliso.chX.400 c=ch; a=400net; p=iso; o=isocs; s=centralPrinted in SwitzerlandiiForewordISO (the International Organization for Standardization) is a worldwidefederation of national standards bodies (ISO member bodies). The work ofpreparing International Standards is normally carried out
5、 through ISOtechnical committees. Each member body interested in a subject for whicha technical committee has been established has the right to be representedon that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collab
6、o-rates closely with the International Electrotechnical Commission (IEC) onall matters of electrotechnical standardization.Draft International Standards adopted by the technical committees arecirculated to the member bodies for voting. Publication as an InternationalStandard requires approval by at
7、least 75 % of the member bodies castinga vote.International Standard ISO 11025 was prepared by Technical CommitteeISO/TC 54, Essential oils.Annex A of this International Standard is for information only.Copyright International Organization for Standardization Provided by IHS under license with ISONo
8、t for ResaleNo reproduction or networking permitted without license from IHS-,-,-ISO ISO 11025:1998(E)iiiIntroductionSince the description of methods of analysis by gas chromatography isvery long, it is considered useful to establish general methods on the onehand, giving detailed information on all
9、 the recurrent parameters, appara-tus, products, methods, formulae, etc., and on the other hand standardswith short details on the determination of specific constituents on the es-sential oils, giving only those operating conditions specific to the pertinentdetermination.This is the case with the pr
10、esent International Standard, which refers to thegeneral standard ISO 7609 for the general paragraphs.Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Copyright Internatio
11、nal Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-INTERNATIONAL STANDARD ISO ISO 11025:1998(E)1Oil of cassia, Chinese type Determination of trans-cinnamaldehyde content Gas chromatographic met
12、hod oncapillary columns1 ScopeThis International Standard specifies a method for thedetermination of the trans-cinnamaldehyde content ofthe essential oil of cassia, Chinese type (Cinna-momum aromaticum Nees, syn. Cinnamomum cassiaNees ex Blume).2 Normative referencesThe following standards contain p
13、rovisions which,through reference in this text, constitute provisions ofthis International Standard. As the time of publication,the editions indicated were valid. All standards aresubject to revision, and parties to agreements basedon this International Standard are encouraged to in-vestigate the po
14、ssibility of applying the most recenteditions of the standards indicated below. Members ofIEC and ISO maintain registers of currently valid Inter-national Standards.ISO 356:1996, Essential oils Preparation of testsamples.ISO 7609:1985, Essential oils Analysis by gaschromatography on capillary column
15、s Generalmethod.3 PrincipleAnalysis by gas chromatography on a capillary col-umn, under specified conditions, of oil of cassia, Chi-nese type. Determination of the trans-cinnamaldehydecontent using the internal standard method.4 Reagents and productsDuring the analysis, unless otherwise specified, u
16、seonly reagents of recognized analytical grade.4.1 Reference substancetrans-Cinnamaldehyde, of purity at least 99 %, deter-mined by chromatography under the test conditions.4.2 Internal standardTridecane, of purity at least 99 %, determined bychromatography under the test conditions.5 Apparatus5.1 C
17、hromatograph, recorder andelectronic integratorSee ISO 7609.5.2 ColumnLength: 25 m to 50 mInternal diameter: 0,2 mm to 0,3 mmStationary phase: polydimethylsiloxane (OV 101) orpolyethylene glycol 20 000(carbowax 20 M)5.3 DetectorFlame ionization type.6 Preparation of test sampleSee ISO 356.7 Operatin
18、g conditions7.1 TemperaturesOven temperature: For example, in the columns, lineartemperature programming from 100 C to 200 C at arate of 3 C/min, or 60 C to 200 C at a rate of1,5 C/min, then kept constant at 200 C for 15 min.Copyright International Organization for Standardization Provided by IHS un
19、der license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-ISO 11025:1998(E)ISO2Injector temperature: For example, 230 C to 240 C.Detector temperature: For example, 230 C to 240 C.7.2 Carrier gas flow rate and auxiliary gasesflow rateSee ISO 7609.8 Column
20、performance8.1 Chemical inertness testCarry out the test as specified in ISO 7609.8.2 Column efficiencyDetermine the column efficiency as specified inISO 7609.9 Determination of retention indexesSee ISO 7609.10 Determination10.1 Determination of response factorDetermine the response factor as specif
21、ied inISO 7609.10.2 Internal standard methodCarry out the determination of the trans-cinnam-aldehyde content of the essential oil by the internalstandard method specified in ISO 7609, using tride-cane (4.2) as internal standard.11 Expression of results11.1 CalculationSee ISO 7609.NOTE Typical chroma
22、tograms are given, for informationonly, in annex A.11.2 RepeatabilitySee ISO 7609.12 Test reportSee ISO 7609.Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-ISOISO 11025:
23、1998(E)3Annex A(informative)Typical chromatograms for determination of the trans-cinnamaldehydecontent in oil of cassia, Chinese typePeak identification1 Styrene2 Benzaldehyde3 Salicylic aldehyde4 Acetophenone5 Phenethyl alcohol6 Dihydrocinnamaldehyde7 cis-Cinnamaldehyde8 trans-Cinnamaldehyde9 trans
24、-Cinnamyl alcohol10 Tridecane (Internal standard)11 Eugenol12 Coumarin13 Cinnamyl acetate14 cis-o-Methoxycinnamaldehyde15 trans-o-Methoxycinnamaldehyde16 o-Methoxycinnamyl acetateOperating conditionsColumn: fused silica capillary, length 50 m, internal diameter0,20 mmStationary phase: polydimethylsi
25、loxane (OV 101)Oven temperature: from 100 C to 200 C, at rate of 3 C/minInjector temperature: 230 CDetector temperature: 230 CVolume injected: 0,2 mlDetector: flame ionizationCarrier gas: nitrogenCarrier gas pressure: 0,4 barSplit ratio: 1/100NOTE The trans-cinnamaldehyde peak should not hide anyoth
26、er peak greater than 0,25 %Figure A.1 Typical chromatogram taken on an apolar columnCopyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-ISO 11025:1998(E)ISO4Peak identificati
27、on1 Tridecane (internal standard)2 trans-CinnamaldehydeOperating conditionsColumn: fused silica capillary, length 60 m, internal diameter 0,25 mmStationary phase: polyethylene glycol 20 000 (carbowax 20 M)Oven temperature: from 60 C to 200 C at a rate of 1,5 C/min, then constant atOven temperature:
28、200 C for 15 minInjector temperature: 240 CDetector temperature: 240 CVolume injected: 0,3 mlDetector: flame ionizationCarrier gas: hydrogenCarrier gas pressure: 0,4 barSplit ratio: 1/100Figure A.2 Typical chromatogram taken on a polar columnCopyright International Organization for Standardization P
29、rovided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IS
30、O 11025:1998(E)ISOICS 71.100.60Descriptors: fruit and vegetable products, essential oils, cassia, chemical analysis, determination of content, gas phase chromatography,chromatograms.Price based on 4 pagesCopyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
