EN 14526:2004

Foodstuffs - Determination of saxitoxin and dc-saxitoxin in mussels - HPLC method using pre-column derivatization with peroxide or periodate oxidation

This European standard specifies a method for the quantitative determination of saxitoxin (STX) and decarbamoyl saxitoxin (dc-STX) in mussels. It may also be applicable in other shellfish, for example scallops. The limit of determination of this method (signal/noise = 10) is 0,006 mg/kg for saxitoxin and 0,02 mg/kg for dc-saxitoxin in mussel meat. The method has been tested for saxitoxin at levels at 0,4 mg/kg and 0,5 mg/kg and for dc-saxitoxin at levels at 0,4 mg/kg and 1,6 mg/kg.

Lebensmittel - Bestimmung von Saxitoxin und DC-Saxitoxin in Muscheln - HPLC-Verfahren mit Vorsäulenderivatisierung mit Peroxid- oder Periodatoxdation

Dieses Dokument legt ein Verfahren für die quantitative Bestimmung von Saxitoxin (STX) und Decarbamoyl-Saxitoxin (DCSTX) in Miesmuscheln fest. Es darf auch auf andere Muscheln angewendet werden, z. B. Jacobsmuscheln. Die Bestimmungsgrenze dieses Verfahrens (Signal/Rauschverhältnis = 10) ist 0,006 mg/kg für Saxitoxin und 0,02 mg/kg für DC-Saxitoxin in Muschelfleisch. Dieses Verfahren wurde im Ringversuch für Saxitoxingehalte von 0,4 mg/kg und 0,5 mg/kg und für DC-Saxitoxingehalte von 0,4 mg/kg und 1,6 mg/kg geprüft.

Produits alimentaires - Détermination de la teneur en saxitoxine et en dc-saxitoxine dans les moules - Méthode par CLHP avec dérivation pré-colonne et par oxydation au peroxide ou au periodate

Le présent document spécifie une méthode de détermination quantitative de la saxitoxine (STX) et de la décarbamoyle saxitoxine (dc-STX) dans les moules. Cette méthode peut également s'appliquer à d'autres mollusques, par exemple les coquilles St-Jacques. La limite de quantification de cette méthode (signal/bruit = 10) est de 0,006 mg/kg pour la saxitoxine et de 0,02 mg/kg pour la dc-saxitoxine dans la chair de moule. Cette méthode a été évaluée pour la saxitoxine aux teneurs de 0,4 mg/kg et 0,5 mg/kg et pour la dc-saxitoxine aux teneurs de 0,4 mg/kg et 1,6 mg/kg.

Živila - Določevanje saksitoksina in dc-saksitoksina v školjkah - Metoda HPLC z uporabo predkolonske derivatizacije s peroksidno ali perjodatno oksidacijo

General Information

• Status: Withdrawn
• Publication Date: 10-Aug-2004
• Withdrawal Date: 17-Jan-2017
• ICS: 67.120.30 - Fish and fishery products
• Technical Committee: CEN/TC 275 - Food analysis - Horizontal methods
• Drafting Committee: CEN/TC 275/WG 14 - Marine Biotoxins
• Current Stage: 9960 - Withdrawal effective - Withdrawal
• Completion Date: 18-Jan-2017
• Ref Project: SIST EN 14526:2005 - Foodstuffs - Determination of saxitoxin and dc-saxitoxin in mussels - HPLC method using pre-column derivatization with peroxide or periodate oxidation

Relations

• Replaced By: EN 14526:2017 - Foodstuffs - Determination of saxitoxin-group toxins in shellfish - HPLC method using pre-column derivatization with peroxide or periodate oxidation
• Effective Date: 06-Jun-2012

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.NVLGDFLMRLebensmittel - Bestimmung von Saxitoxin und DC-Saxitoxin in Muscheln - HPLC-Verfahren mit Vorsäulenderivatisierung mit Peroxid- oder PeriodatoxdationProduits alimentaires - Détermination de la teneur en saxitoxine et en dc-saxitoxine dans les moules - Méthode par CLHP avec dérivation pré-colonne et par oxydation au peroxide ou au periodateFoodstuffs - Determination of saxitoxin and dc-saxitoxin in mussels - HPLC method using pre-column derivatization with peroxide or periodate oxidation67.120.30Ribe in ribji proizvodiFish and fishery productsICS:Ta slovenski standard je istoveten z:EN 14526:2004SIST EN 14526:2005en01-januar-2005SIST EN 14526:2005SLOVENSKI
STANDARD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14526August 2004ICS 67.120.30English versionFoodstuffs - Determination of saxitoxin and dc-saxitoxin inmussels - HPLC method using pre-column derivatization withperoxide or periodate oxidationProduits alimentaires - Détermination de la teneur ensaxitoxine et en dc-saxitoxine dans les moules - Méthodepar CLHP avec dérivation pré-colonne et par oxydation auperoxide ou au periodateLebensmittel - Bestimmung von Saxitoxin und DC-Saxitoxinin Muscheln - HPLC-Verfahren mitVorsäulenderivatisierung mit Peroxid- oderPeriodatoxdationThis European Standard was approved by CEN on 21 May 2004.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2004 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14526:2004: ESIST EN 14526:2005

Performance data.16 Bibliography.17
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. WARNING — The use of this standard can involve hazardous materials, operations and equipment. This standard does not purport to address all the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. SIST EN 14526:2005

second + dc-STX oxid. (2)
third ++ STX oxid. dc-STX first ++ dc-STX oxid. (1)
second + dc-STX oxid. (2)
The method described in this document is suitable for the quantitative determination of the PSP toxins STX and dc-STX. The following should however be considered. Co-occurrence of different PSP toxins in mussels could influence the analytical results, because some of the PSP toxins could (partially) lead to the same reaction products. So the chromatograms shall be carefully interpreted. The analytical result obtained for STX with hydrogen peroxide oxidation is not influenced by the presence of other toxins. SIST EN 14526:2005

= 30 % with 2 ml of water. Store cool and in the dark. Prepare fresh every week. 4.8 Periodic acid solution, c = 0,03 mol/l Dissolve 0,68 g of periodic acid in 100 ml of water. 4.9 Disodium hydrogenphosphate solution, c = 0,3 mol/l Dissolve 0,53 g of disodium hydrogenphosphate dihydrate in 10 ml of water. 4.10 Acetic acid, 100 % 4.10.1 Acetic acid solution 1, c = 1 mol/l Dilute 57,2 ml of acetic acid solution (4.10) to 1,0 l with water. 4.10.2 Acetic acid solution 2, c = 0,1 mol/l Dilute 10 ml of acetic acid solution 1 (4.10.1) with 90 ml of water. 4.10.3 Acetic acid solution 3, c = 0,2 mol/l Dilute 200 ml of acetic acid solution 1 (4.10.1) with 800 ml of water. 4.10.4 Acetic acid solution 4, c = 0,03 mol/l Dilute 300 ml of acetic acid solution 2 (4.10.2) with 700 ml of water. 4.11 Helium 4.12 Peroxide derivatization reagent Dilute 400 µl of hydrogen peroxide solution (4.7) with 4 ml of sodium hydroxide solution 2 (4.6.2) and mix well. Prepare fresh every day of analysis. 4.13 Periodate derivatization reagent Mix 1 volume part of periodic acid solution (4.8) with 1 volume part of disodium hydrogenphosphate solution (4.9) and 1 volume part of ammonium formate solution 1 (4.4.1). Bring the mixture to about pH 8 by dropwise adding sodium hydroxide solution 2 (4.6.2) and check the pH by using pH paper. Prepare fresh every day of analysis just before use. SIST EN 14526:2005

= 1,0 µg/ml Prepare a stock solution containing 1,0 µg/ml of saxitoxin in acetic acid solution 4 (4.10.4) by weighing with the analytical balance (5.3). Store the solution cool (approximately + 4 °C) and in the dark. This solution is stable for at least 5 months (see [6]). NOTE Ampoules containing saxitoxin (STX·2HCl) standard are for example available from the National Research Council Canada, Halifax, Canada (set of calibrants PSP-1) 1) . 4.14
...