ISO-13493-1998.pdf
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1、A Reference number ISO 13493:1998(E) INTERNATIONAL STANDARD ISO 13493 First edition 1998-09-01 Meat and meat products Determination of chloramphenicol content Method using liquid chromatography Viande et produits base de viande Dosage du chloramphnicol Mthode par chromatographie en phase liquide Cop
2、yright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:11:59 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13493:1998(E) ISO 1998 All rights reserved. Un
3、less 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. International Organization for Standardization Case postale 56 CH-1211 Ge
4、nve 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 International Standards is normally carried out through ISO technical com
5、mittees. 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 with th
6、e International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. 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 m
7、ember bodies casting a vote. International Standard ISO 13493 was prepared by Technical Committee ISO/TC 34, Agricultural food products, Subcommittee SC 6, Meat and meat products. Annex A of this International Standard is for information only. Copyright International Organization for Standardization
8、 Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:11:59 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISOISO 13493:1998(E) 1 Meat and meat products Determination of chloramphenicol c
9、ontent Method using liquid chromatography 1 Scope This International Standard specifies a liquid chromatographic method for the determination of the chloramphenicol content of the muscle tissue of meat, including poultry. The method is suitable for the determination of chloramphenicol contents great
10、er than 6,5 g/kg. Test samples which have deteriorated cannot be analysed with this method. NOTE This International Standard may be applicable for the determination of the chloramphenicol content of all kinds of meat and meat products. However, materials other than muscle tissue were not included in
11、 the collaborative testing of the method. 2 Normative reference The following standard contains provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the edition indicated was valid. All standards are subject to revision,
12、and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent edition of the standard indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 3696:1987, Water for analytical
13、laboratory use Specification and test methods. 3 Definition For the purposes of this International Standard, the following definition applies. 3.1 chloramphenicol content of meat and meat products mass fraction of chloramphenicol residue determined according to the procedure specified in this Intern
14、ational Standard. NOTE The chloramphenicol content is expressed in micrograms per kilogram. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:11:59 MDTNo reproduction or network
15、ing permitted without license from IHS -,-,- ISO 13493:1998(E) ISO 2 4 Principle A test portion is extracted with water. Filtration and solid-phase extraction are used to isolate the lipophilic components from the aqueous solution. The chloramphenicol is eluted from the cartridge with dichloromethan
16、e. The organic phase is evaporated and purified by liquid-liquid extraction with water and toluene. The chloramphenicol is measured with reverse-phase chromatography by ultraviolet (UV) detection. 5 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. 5.1 Water, com
17、plying with at least grade 3 in accordance with ISO 3696. The water shall be free of organic compounds. 5.2 Nitrogen, suitable for evaporating solvents. 5.3 Dichloromethane. 5.4 Toluene. 5.5 Acetate buffer, c(CH3CO2Na) = 0,01 mol/l, pH = 4,3. Dissolve 0,82 g of anhydrous sodium acetate in about 970
18、ml of water. Adjust the pH to 4,3 with 50 % (m/m) dilute acetic acid (CH3CO2H) using the pH-meter (6.1). Transfer the solution to a 1000 ml one-mark volumetric flask. Dilute to the mark with water and mix. 5.6 Acetonitrile, suitable for UV spectroscopy. 5.7 Mobile phase. Add 750 ml of acetate buffer
19、 (5.5) to 250 ml of acetonitrile (5.6) and mix thoroughly. Before use, filter the eluent through a 0,22 mm filter (6.2) and degas. 5.8 Chloramphenicol stock solution, 100 mg/ml. Weigh, to the nearest 0,1 mg, 10 mg of chloramphenicol and transfer it to a 100 ml one-mark volumetric flask. Dilute to th
20、e mark with methanol and mix. This stock solution is stable for 1 month when stored in the dark. 5.9 Chloramphenicol standard solutions. Pipette 5,0 ml of the stock solution (5.8) into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix. Prepare four standard solutions by dilut
21、ing 1,0 ml, 2,0 ml, 5,0 ml and 15,0 ml of this solution to 100 ml with water to obtain solutions with a chloramphenicol content of 0,05 mg/ml, 0,10 mg/ml, 0,25 mg/ml and 0,75 mg/ml respectively. These standard solutions are stable for 1 week when stored in the dark. 6 Apparatus Usual laboratory appa
22、ratus and, in particular, the following. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:11:59 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO IS
23、O 13493:1998(E) 3 6.1 pH-meter. 6.2 Membrane filter, of low dead volume and pore size 0,22 mm. 6.3 Mechanical or electrical equipment capable of homogenizing the laboratory sample. This includes a high-speed rotational cutter, or a mincer fitted with a plate with apertures not exceeding 4,0 mm in di
24、ameter. 6.4 Laboratory blender (e.g. Stomacher blender 1) or vortex type). 6.5 Filter paper, quantitative, fast filtration rate, of diameter about 15 cm. NOTEFor example, Whatman 41 proved to be suitable 1). 6.6 Extraction cartridges, of capacity 20 ml, containing diatomaceous earth that extracts li
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