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1、BRITISH STANDARD BS ISO 18054:2004 Oils of orris rhizome (Iris pallida Lam. or Iris germanica L.) Determination of irone content Method using gas chromatography on a capillary column ICS 71.100.60 ? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:12:38 GMT+00:00 2006, Uncontrolled Copy, (c
2、) BSI BS ISO 18054:2004 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 1 June 2004 BSI 1 June 2004 ISBN 0 580 43837 6 National foreword This British Standard reproduces verbatim ISO 18054:2004 and implements it as the UK national standard. T
3、he UK participation in its preparation was entrusted to Technical Committee AW/54, Essential oils, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international
4、publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all th
5、e necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on th
6、e interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 8, an in
7、side back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:12:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Refe
8、rence number ISO 18054:2004(E) INTERNATIONAL STANDARD ISO 18054 First edition 2004-05-15 Oils of orris rhizome (Iris pallida Lam. or Iris germanica L.) Determination of irone content Method using gas chromatography on a capillary column Huile essentielle de rhizomes diris (Iris pallida Lam. ou Iris
9、germanica L.) Dtermination de la teneur en irones Mthode par chromatographie en phase gazeuse sur colonne capillaire BS ISO 18054:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:12:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI DPlcsid Fremia ihTs PDF file mya ctnoian emdebt dedyfepcae
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13、 Mon Nov 27 04:12:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technica
14、l 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-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely wit
15、h 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. The main task of technical committees is to prepare International Standards. Draft Inter
16、national 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 vote. Attention is drawn to the possibility that some of the elements of this document may
17、 be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 18054 was prepared by Technical Committee ISO/TC 54, Essential oils. BS ISO 18054:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:12:38 GMT+00:00 2006, Uncontrolled C
18、opy, (c) BSI iv Introduction Since the description of methods of analysis by gas chromatography is very long, it is considered useful to establish general methods giving detailed information on all the recurrent parameters, apparatus, products, methods, formulae, etc. and then standards with short d
19、etails on the determination of specific constituents in essential oils, giving only those operating conditions specific to the pertinent determination. This is the case with the present International Standard, which refers to the general standard ISO 7609 for the general paragraphs. BS ISO 18054:200
20、4 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:12:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 1 Oils of orris rhizome (Iris pallida Lam. or Iris germanica L.) Determination of irone content Method using gas chromatography on a capillary column 1 Scope This International Standard speci
21、fies a method for the determination of irone content in oils of orris1) rhizome (Iris pallida Lam. or Iris germanica L.) using gas chromatography on a capillary column. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated referen
22、ces, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 356, Essential oils Preparation of test samples ISO 7609, Essential oils Analysis by gas chromatography on capillary columns General method 3 Principle G
23、as phase chromatography on small quantities of orris essential oils is carried out on a capillary column, under the specified analytical conditions. The irone content is determined by the internal standard method. 4 Reagents and products 4.1 Reference substance: synthetic irones of which the sum of
24、the isomers is greater than 90 %, determined by chromatography under the test conditions. 4.2 Internal standard Select either one of the following recently distilled substances, depending on whether a polar or apolar column is being used. The internal standard selected shall elute as near as possibl
25、e to the compound(s) to be determined, and shall not overlap any of the peaks corresponding to the constituents of the essential oil in question. 4.2.1 -Ionone, having a minimum purity of 98 %, determined by gas chromatography under the test conditions, for determination on a polar column. 4.2.2 tra
26、ns-Anethole, having a minimum purity of 98 %, determined by gas chromatography under the test conditions, for determination on an apolar column. 1) Commercially, this is usually called “orris butter”. BS ISO 18054:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:12:38 GMT+00:00 2006, U
27、ncontrolled Copy, (c) BSI 2 4.3 Dilution solvent: dichloromethane, having a minimum purity of 99 %, determined by gas chromatography under the test conditions, or any other suitable solvent, of identical analytical quality. WARNING Attention is drawn to the hazards of using dichloromethane, which is
28、 a toxic solvent. 4.4 Additive substance: linalool, having a minimum purity of 99 %, determined by chromatography under the test conditions. 5 Apparatus 5.1 Chromatograph, recorder and integrator. See ISO 7609. 5.2 Column. Capillary column having the characteristics given in 5.2.1 and 5.2.2. 5.2.1 P
29、olar capillary column. Length 10 m to 100 m Internal diameter 0,2 mm to 0,5 mm Stationary phase poly(ethylene glycol) 20 000 (FFAP, Supelcowax), for example 5.2.2 Apolar capillary column. Length 10 m to 100 m Internal diameter 0,2 mm to 0,5 mm Stationary phase methyl silicone, for example 5.3 Flame
30、ionization detector. 6 Preparation of test sample See ISO 356. 7 Operating conditions 7.1 Temperatures 7.1.1 Oven temperature The oven temperature shall be chosen so that the irone isomers are well separated from the other essential oil constituents. The following temperatures are given by way of in
31、dication. a) Polar capillary column Linear temperature programming from 100 C to 220 C, at a rate of 2 C/min to 3 C/min. BS ISO 18054:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:12:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 3 b) Apolar capillary column Linear temperature progra
32、mming from 100 C to 250 C, at a rate of 2 C/min to 3 C/min. 7.1.2 Injection temperature About 230 C. 7.1.3 Detection temperature a) Polar capillary column About 230 C. b) Apolar capillary column About 260 C. 7.2 Carrier gas and auxiliary gases flow rates See ISO 7609. 8 Column performance 8.1 Chemic
33、al inertness test Carry out the test as specified in ISO 7609. 8.2 Column efficiency Determine the efficiency of the column as specified in ISO 7609. The efficiency shall be at least 50 000 theoretical plates, determined on the linalol peak, under the test conditions. The irone isomers shall be well
34、 separated. 9 Determination of retention indexes See ISO 7609. 10 Identification of the irone isomers See the typical chromatograms given in Annex A. 11 Determination by internal standard method 11.1 Determination of the response factor Determine the response factor in accordance with ISO 7609, usin
35、g the irone (4.1) as the reference substance and either a) or b) of the following standard mixtures, depending on whether the determination is conducted on a polar or an apolar capillary column. Prepare the standard mixtures by weighing, taking into account the analytical purity of the standards in
36、the calculation of the masses of the weighed products. BS ISO 18054:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:12:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 4 a) Standard mixture for polar capillary column -Ionone (4.2.1) 0,1 g Synthetic irones 0,1 g Linalool (4.4) 0,8 g Dichl
37、oromethane (4.3) 4 g approximately b) Standard mixture for apolar capillary column trans-Anethole (4.2.2) 0,1 g Synthetic irones 0,1 g Linalool (4.4) 0,8 g Dichloromethane (4.3) 4 g approximately NOTE 1 The purpose of adding linalool to the standard mixtures is to obtain irone concentrations close t
38、o those of the synthetic irones. NOTE 2 The weighing accuracy given in ISO 7609 is not applicable to the dilution solvent dichloromethane (4.3). A relative weighing accuracy of 5 % suffices. NOTE 3 For the calculation of the response factor, K, AR is the sum of the areas of the peaks of the referenc
39、e irone isomers. It is assumed that the response factors of the isomers are identical. 11.2 Determination of the irones in the sample Carry out a determination of the irone content of the essential oil being analysed in accordance with the internal standard method specified in ISO 7609, using either
40、 a) or b) of the following test mixtures, depending on whether a polar or an apolar capillary column is used. Prepare the mixtures by weighing. a) Test mixture for polar capillary column -Ionone (4.2.1) 0,1 g Synthetic irones 0,9 g Dichloromethane (4.3) 4 g approximately b) Test mixture for apolar c
41、apillary column trans-Anethole (4.2.2) 0,1 g Synthetic irones 0,9 g Dichloromethane (4.3) 4 g approximately NOTE 1 The weighing accuracy given in ISO 7609 is not applicable to the dilution solvent dichloromethane (4.3). A relative weighing accuracy of 5 % suffices. NOTE 2 For the determination of th
42、e irone content of the synthetic irones, Ax is the sum of the areas of the peaks of the irone isomers. It is assumed that the response factors of the isomers are identical. BS ISO 18054:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:12:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 5
43、12 Expression of results See ISO 7609. NOTE Typical chromatograms of the analysis are given in Annex A, for information. 13 Precision 13.1 Interlaboratory test Details of an interlaboratory test on the precision of the method are summarized in Annex B. 13.2 Repeatability The absolute difference betw
44、een two independent single test results, obtained using the same method on identical test material in the same laboratory by the same operator using the same equipment within a short interval of time, should not be greater than 5 %. 13.3 Reproducibility The absolute difference between two single tes
45、t results, obtained using the same method on identical test material in different laboratories with different operators using different equipment, should not be greater than 10 %. 14 Test report See ISO 7609. BS ISO 18054:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:12:38 GMT+00:00
46、 2006, Uncontrolled Copy, (c) BSI 6 Annex A (informative) Typical chromatograms of the determination by gas chromatography of the irone content in the oil of orris rhizome (Iris pallida Lam. or Iris germanica L.), of Moroccan origin A.1 Identification of irone isomers and determination of the respon
47、se factor on an apolar phase standard mixture 11.1 b) Peak identification Operating conditions 1 Dichloromethane 2 Linalool 3 trans-Anethole 4 trans-Irone 5 cis-Irone 6 cis-Irone 7 -Irone Column: quartz capillary; length 50 m; internal diameter 0,32 mm Stationary phase: poly(dimethyl siloxane) (CPSi
48、l 5 CB) Film thickness: 0,4 m Oven temperature: temperature programming from 100 C to 270 C at a rate of 2 C/min Injector temperature: 230 C Detector temperature: 250 C Detector: flame ionization type Carrier gas: helium Volume injected: 1 l Carrier gas flow rate: 1 ml/min Figure A.1 Typical chromat
49、ogram taken on an apolar column BS ISO 18054:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:12:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 7 A.2 Identification of irones on an apolar phase test mixture 11.2 b) Peak identification Operating conditions 1 Dichloromethane 2 trans-Anethole 3 trans-Irone 4 cis-Irone 5 cis-Irone 6 -Irone 7 Myristic acid Column: quartz capillary; length 50 m; internal diameter 0,32 mm Stationary