1、BRITISH STANDARD BS ISO 22972:2004 Essential oils Analysis by gas chromatography on chiral capillary columns General method ICS 71.100.60 BS ISO 22972:2004 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 4 June 2004 BSI 4 June 2004 ISBN 0 580
2、 43839 2 National foreword This British Standard reproduces verbatim ISO 22972:2004 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee AW/54, Essential oils, which has the responsibility to: A list of organizations represented
3、on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international 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 “
4、Search” facility of the BSI Electronic Catalogue or of British Standards Online. This 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 does not of itself confer immunity from lega
5、l obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Su
6、mmary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 4, an inside 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 A
7、md. No. Date Comments Reference number ISO 22972:2004(E) OSI 4002INTERNATIONAL STANDARD ISO 22972 First edition 2004-05-15 Essential oils Analysis by gas chromatography on chiral capillary columns General method Huiles essentielles Analyse par chromatographie en phase gazeuse sur colonne capillaire
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13、2 O4002(E) I SO 4002 All irthgs ersedevr iiiForeword 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 technical committees. Each membe
14、r 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 with the International Elec
15、trotechnical 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 International Standards adopt
16、ed 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 be the subject of paten
17、t rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 22972 was prepared by Technical Committee ISO/TC 54, Essential oils. BSISO22972:2004ISO 22972:2004(E) iv I SO 4002 All irthgs ersedevrIntroduction Since the description of gas chromatographic analysis meth
18、ods is long, it has been considered worthwhile to draw up general standards giving detailed information on all the recurrent parameters (apparatus, products, methods, calculation formulae, etc.), and then short-version standards (abridged analysis sheets) relating to the determination of the enantio
19、meric excess or distribution of chiral compounds present in essential oils. This is the case with this International Standard, which makes reference to ISO 7609 for the general clauses. BSISO22972:2004INTENRATIONAL TSANDADR IS:27922 O4002(E)I SO 4002 All irthgs ersedevr 1Essential oils Analysis by g
20、as chromatography on chiral capillary columns General method 1 Scope This International Standard specifies a general method for the analysis of essential oils by gas chromatography on capillary chiral columns, for the purpose of determining the specific enantiomeric excess or distribution of the chi
21、ral compounds contained in the essential oils. 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
22、amendments) applies. ISO 356, Essential oils Preparation of test samples ISO 7609:1985, Essential oils Analysis by gas chromatography on capillary columns General method 3 Principle The essentail oil is analysed by gas chromatography, under specified analytical conditions, on a column of appropriate
23、 diameter and length, the inside wall of this column having been previously impregnated, either directly with a bonded chiral stationary phase or with a support of this stationary phase. The different chiral constituents of interest in the essential oil are indentified with respect to standard subst
24、ances and, if necessary, by measurement of their retention index and determination of the relative proportions of the enantiomers of a constituent. 4 Reagents and products During the course of the analysis, unless otherwise specified, use only reagents of recognized analytical grade. 4.1 Gas. 4.1.1
25、Carrier gas: hydrogen, helium or nitrogen, or any other gas, depending on the type of detector being used. If a detector requiring a carrier gas other than those mentioned is used, this should be stated in the test report. 4.1.2 Detector supply gas: all suitable gases, depending on the detector bein
26、g used: for a flame ionization detector, air and hydrogen of high purity; for a mass detector, helium of high purity. 4.2 Reference substance, corresponding to the pure and mixed enantiomers to be detected. BSISO22972:2004ISO 22972:2004(E) 2 I SO 4002 All irthgs ersedevr5 Apparatus 5.1 Chromatograph
27、, equipped with an injection system, an appropriate detector and a temperature programmer. The injection and detection systems shall be fitted with devices for independent control of their respective temperatures. 5.2 Capillary column, made of an inert material, having an inner diameter u 0,53 mm an
28、d a length between 10 m and 60 m. NOTE Common chiral stationary phases are based on substituted -cyclodextrins (e.g. 1,3,6-permethylated -cyclodextrin at 10 % in OV 101 ). 5.3 Recorder and electronic integrator. 6 Preparation of the test sample See ISO 356. The test sample may have to undergo the fo
29、llowing special preparation: selective transfer of the relevant constituent(s) (e.g. in-line two-dimensional chromatography or trapping); derivatization prior to injection. If it is the case, this will be mentioned in the standard on the relevant essential oil. 7 Operating conditions 7.1 Oven temper
30、ature The oven temperature shall be regulated in such a way as to obtain the required efficiency (see 8.1). 7.2 Carrier gas flow rate The flow rate shall be regulated in such a way as to obtain the required efficiency (see 8.1). 7.3 Flow rate of detector supply gases Refer to the appliance manufactu
31、rers instructions in order to obtain the optimum response from the detector. 8 Column performance 8.1 Column efficiency Determine the column efficiency on the less-retained enantiomer of the selected reference substance (see 4.2), according to the method described in ISO 7609. The efficiency shall b
32、e at least 25 000 theoretical plates. NOTE When a two-dimensional chromatographic system is used, the temperature programming conditions can be optimized for each component of interest (or chemical family), so as to obtain a satisfactory resolution with a reduced analysis time. In this case, the eff
33、icacy may be lower than 25 000 theoretical plates. BSISO22972:2004ISO 22972:2004(E) I SO 4002 All irthgs ersedevr 38.2 Resolution and separation Determine the resolution by injecting a quantity of the selected reference substance (see 4.2) under the test conditions. Carry out the calculations in acc
34、ordance with ISO 7609:1985, 8.3.1 and 8.3.2. The injection of the reference substance under analysis conditions shall not lead to any deterioration of the enantiomers or to any variation in their ratio. 9 Determination of the retention indexes See ISO 7609. NOTE When a two-dimensional chromatographi
35、c system is used, the determination of the retention indexes is optional if the conditions of elution on both chromatographs and the resolution of the enantiomer are similar to those of the reference substances, within the random variations. 10 Determination of the enantiomeric excess or distributio
36、n Use the same temperature and flow rate conditions as those adopted for the column efficiency test (see 8.1). After stabilization of the column temperature, inject an appropriate quantity of the test portion. On the obtained essential oil chromatogram, verify, using the indications provided by the
37、integrator, compliance with the limits set out in the standards specific to the relevant essential oil. Particularly in the case of use of a mono-dimensional chromatographic system, it is recommended to verify by all appropriate means (e.g. mass detector) the absence of co-elution for the substances
38、 being sought. 11 Expression of results 11.1 General Express the results either in enantiomeric excess or in enantiomeric distribution in accordance with the requirements of the standard specific to the relevant essential oil. 11.2 Enantiomeric excess: E Determine the enantiomeric excess, E, from th
39、e area of each of the enantiomer peaks: max min max min () 100 () x AA E AA = +where x = (R) if max A is for enantiomer (R); x = (S) if max A is for enantiomer (S); max A is the peak area presenting the largest surface; min A is the peak area presenting the smallest surface. BSISO22972:2004IS:27922
40、O4002(E) 4 I SO 4002 All irthgs ersedevr11.3 Enantiomeric distribution (R) (R) % 100 (R) (S) A AA = +(S) (S) % 100 (R) (S) A AA = +where (R) A is the enantiomer (R) peak area; (S) A is the enantiomer (S) peak area. In the event of the enantiomeric excess or distribution being respectively greater th
41、an 95 % or 97,5 %, it is recommended to pay particular attention to the choice of the integration parameters in order to minimize the error on the quantification of the least abundant enantiomer. The latter will be quantified, as far as possible, under acceptable chromatographic resolution condition
42、s. 12 Test report See ISO 7609. BSISO22972:2004BS ISO 22972:2004 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.
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