ISO-11023-1999.pdf
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1、A Reference number ISO 11023:1999(E) INTERNATIONAL STANDARD ISO 11023 First edition 1999-10-15 Liquorice extracts (Glycyrrhiza glabra L.) Determination of glycyrrhizic acid content Method using high-performance liquid chromatography Extraits de rglisse (Glycyrrhiza glabra L.) Dtermination de la tene
2、ur en acide glycyrrhizique Mthode par chromatographie liquide haute performance Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:13:25 MDTNo reproduction or networking permitted without license
3、 from IHS -,-,- ISO 11023:1999(E) ISO ISO 1999 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. Int
4、ernational Organization for Standardization Case postale 56 CH-1211 Genve 20 Switzerland Internetisoiso.ch Printed in Switzerland ii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Int
5、ernational 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-governmental, in liaison w
6、ith 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 3. Draft International Sta
7、ndards 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. International Standard ISO 11023 was prepared by Technical Committee ISO/TC 54, Essential oils.
8、Annex A of this International Standard is for information only. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:13:25 MDTNo reproduction or networking permitted without license from IHS -,-,-
9、INTERNATIONAL STANDARD ISOISO 11023:1999(E) 1 Liquorice extracts (Glycyrrhiza glabra L.) Determination of glycyrrhizic acid content Method using high-performance liquid chromatography 1 Scope This International Standard describes a method for determining the glycyrrhizic acid content of liquorice ex
10、tract (Glycyrrhiza glabra L.) by high-performance liquid chromatography. The method is not applicable to raw or ground liquorice root. 2 Principle The sample and standard solutions are prepared, then the glycyrrhizic acid content is determined by high- performance liquid chromatography using the met
11、hod described in this International Standard. 3 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. 3.1 Water, HPLC grade. 3.2 Reference substance, monoammoniacal glycyrrhizate (GMA). If a reference material of guaranteed purity is not available, it is recommended
12、that the users of this International Standard come to an agreement between the interested parties on the purity of the reference substance. 3.3 Acetonitrile, HPLC grade. 3.4 Acetic acid, analytical grade. 3.5 Elution solvent (mobile phase), composed of the following: 38 volumes acetonitrile (3.3), 6
13、1 volumes water (3.1), 1 volume acetic acid (3.4). Using the measuring cylinder (4.3), prepare the elution solvent as follows. Mix 1 volume of acetic acid with 61 volumes of water, then filter the mixture through a filter for aqueous solvents (4.5). Filter 38 volumes of acetonitrile through a filter
14、 for organic solvents (4.4). Add the filtered acetonitrile to the filtered water/acetic acid mixture. Mix, then degas the elution solvent in the ultra- sound cell (4.8.3) or any suitable system. Do not keep this solvent more than 48 h at ambient temperature. Copyright International Organization for
15、Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:13:25 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11023:1999(E) ISO 2 4 Apparatus Usual laboratory apparatus and, in particular, the following. 4.1 Pip
16、ettes, of capacities 5 ml and 10 ml. 4.2 Volumetric flasks, of capacities 50 ml and 100 ml. 4.3 Measuring cylinder. 4.4 Filter for organic solvents, 0,5 m pore size. 4.5 Filter for aqueous solvents, 0,45 m pore size. 4.6 Oven, capable of being maintained at 105 C + 2 C. 4.7 Analytical balance, capab
17、le of weighing to the nearest 0,000 1 g. 4.8 Separation system, as follows. 4.8.1 Chromatograph, high-performance liquid phase. 4.8.2 Pumping system, for obtaining and maintaining a constant or programmed high pressure flow. 4.8.3 Solvent degassing system, such as an ultra-sound cell or any suitable
18、 system. 4.8.4 Ultraviolet detection system, adjustable to a wavelength of 254 nm. 4.9 Recorder or integrator, of compatible performance with all the apparatus. 4.10 Column, as follows: material: stainless steel or glass; length: 10 cm to 25 cm; internal diameter: 0,4 cm to 0,5 cm; stationary phase:
19、 bonded phase silica with octadecyl C18 derived functional group, maximum particle size 5 mm; column efficiency: the number recommended of theoretical plates is 7 000 to 10 000. 4.11 Pre-column, as follows: material: stainless steel; length: 10 mm or 25 mm; internal diameter: 2 mm or 4 mm; stationar
20、y phase: bonded phase silica with octadecyl C18 derived functional group Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:13:25 MDTNo reproduction or networking permitted without license from I
21、HS -,-,- ISOISO 11023:1999(E) 3 5 Procedure 5.1 Preparation of standard solutions 5.1.1 Preparation of the 0,5 mg/ml solution In a 100 ml volumetric flask (4.2) weigh, to the nearest 104 g, 50 mg of monoammoniacal glycyrrhizate (3.2). Add the elution solvent (3.5) and dissolve the monoammoniacal gly
22、cyrrhizate (3.2). Make up to the mark with a further quantity of elution solvent. Filter if necessary through the organic solvent filter (4.4). It is essential to prepare a new solution every day. 5.1.2 Preparation of dilute solutions containing 0,05 mg/ml, 0,075 mg/ml and 0,1 mg/ml 5.1.2.1 0,05 mg/
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