ISO 20179-2005 Water quality - Determination of microcystins - Method using solid phase extraction (SPE) and high performance liquid chromatography (HPLC) with .pdf
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1、 Reference number ISO 20179:2005(E) ISO 2005INTERNATIONAL STANDARD ISO 20179 First edition 2005-10-01 Water quality Determination of microcystins Method using solid phase extraction (SPE) and high performance liquid chromatography (HPLC) with ultraviolet (UV) detection Qualit de leau Dosage des micr
2、ocystines Mthode utilisant lextraction en phase solide (SPE) et la chromatographie en phase liquide haute performance (CLHP) avec dtection dans lultraviolet (UV) ISO 20179:2005(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may b
3、e printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobes licensing policy. The ISO Central Secretariat accepts
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5、ile is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. ISO 2005 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any for
6、m or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09
7、47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2005 All rights reservedISO 20179:2005(E) ISO 2005 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references . 1 3 Abbreviated terms 1 4 Principle. 2 5 Reagents 2 6 Apparatus 5 7 Proc
8、edure 6 8 Method performance characteristics and data 10 9 Test report . 10 Annex A (informative) Mass spectrometry (MS) as an alternative detection . 11 Annex B (informative) Typical chromatogram and absorption spectra . 14 Annex C (informative) Precision data. 16 Bibliography . 17 ISO 20179:2005(E
9、) iv ISO 2005 All rights reservedForeword 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 member body inte
10、rested 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 Electrotechnica
11、l 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 adopted by the t
12、echnical 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 patent rights. I
13、SO shall not be held responsible for identifying any or all such patent rights. ISO 20179 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. ISO 20179:2005(E) ISO 2005 All rights reserved v Introduction The user should be awa
14、re that particular problems could require the specification of additional conditions. INTERNATIONAL STANDARD ISO 20179:2005(E) ISO 2005 All rights reserved 1 Water quality Determination of microcystins Method using solid phase extraction (SPE) and high performance liquid chromatography (HPLC) with u
15、ltraviolet (UV) detection WARNING The method requires use of microcystin-containing solutions. Microcystins are highly hepatotoxic to humans. Laboratory wastes of microcystins shall be collected separately and disposed as highly toxic chemical waste. Long-term decontamination with concentrated sodiu
16、m hypochlorite (NaClO) solution is also possible. Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish app
17、ropriate safety and health practices and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted according to this standard be carried out by suitably trained staff. 1 Scope This International Standard specifies a method for the determi
18、nation and quantification of microcystins in raw water (containing biomass) and treated water, such as tap water. The method described is validated for MCYST-RR, MCYST-YR, and MCYST-LR. It is also applicable for the determination of several structure variants 1of these microcystins, but an unambiguo
19、us identification cannot be made due to the lack of commercially available standards and due to co-elution. The threshold value of 1 g/l of MCYST-LR in water, proposed by the World Health Organization, can be followed after microcystin enrichment using solid phase extraction (SPE). 2 Normative refer
20、ences 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 amendments) applies. ISO 3696:1987, Water for analytical laborat
21、ory use Specification and test methods ISO 5667-4, Water quality Sampling Part 4: Guidance on sampling from lakes, natural and man-made ISO 5667-5, Water quality Sampling Part 5: Guidance on sampling of drinking water from treatment works and piped distribution systems 3 Abbreviated terms For the pu
22、rposes of this document, the following abbreviated terms apply. APCI atmospheric pressure chemical ionization MCYST microcystin MCYST-LR microcystin containing leucine (L) and arginine (R) ISO 20179:2005(E) 2 ISO 2005 All rights reservedMCYST-RR microcystin containing two arginine (R) units MCYST-YR
23、 microcystin containing tyrosine (Y) and arginine (R) SIM selected ion monitoring SEC size exclusion chromatography 4 Principle Water samples containing cyanobacterial material (biomass) shall be filtered first. The biomass is extracted separately with a solvent (methanol/water). The extract is filt
24、ered, diluted and a solid phase extraction (SPE) is applied for sample clean-up. The filtrate is treated as a pure water sample (see below). Pure water samples such as tap water are enriched using SPE. The microcystins are eluted from the SPE cartridges with methanol/water 90/10 by volume containing
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