Lyophilised samples of blank urine for the validation and quality control of residue analysis for growth promoting compounds
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Series / Report no.
Open Access
Type
Report
Language
en
Date
1998-11-12
Research Projects
Organizational Units
Journal Issue
Title
Lyophilised samples of blank urine for the
validation and quality control of residue analysis for growth promoting
compounds
Translated Title
Gevriesdroogde monsters blanco urine voor de
validatie en kwaliteits controle van de residu analyse op groei-bevorderende
stoffen
Published in
Abstract
Voor het opzetten van een collectie (bank) van
referentiemonsters blanco urine werden vijftig verschillende monsters in
kleine hoeveelheden (5 ml) gevriesdroogd. Voor runderen, schapen en varkens
zijn van 10 tot 20 verschillende dieren monsters urine verzameld. De
individuele dieren verschilden in ras en geslacht en werden gevoerd met
verschillende types voeder. Na vriesdrogen werd een uitgebreide serie
kwaliteits controle testen uitgevoerd. Variatie in de netto gewichten van
de urines en de gevriesdroogde droogresten, werden voor een percentage van
de flesjes van iedere batch bepaald. Voor de meeste batches was de
spreiding voor urines en droogresten respectievelijk niet groter dan 0.1%
en 1%. Het rest gehalte aan water voor elke batch na het vriesdrogen werd
bepaald d.m.v. een Karl-Fisher titratie. Het percentage rest water
varieerde voor de monsters runderurine van 1.0-7.0%, voor de monsters
varkens urine van 1.3-3% en voor de monsters schapen urine van 1.6-5.5%.
In 10 van de 50 batches is het rest water percentage hoger dan de van te
voren beoogde 5%. Elke batch is geanalyseerd op de aanwezigheid van
anabolica met een multi residu methode ontwikkeld bij ARO/CRL. In 2
monsters runder urine werd de aanwezigheid van a-boldenon bevestigd. In de
meeste monsters varkens- en schapen- urine werden het endogene a-testosteron
en a-estradiol aangetoond. In een aantal monsters varkens- en schapen-urine
werden a- en b-zearalenol, metabolieten van het fusarium toxine zearalenon,
aangetoond. De setjes gevriesdroogde monsters blanco urine worden
beschikbaar gesteld aan officiele controle laboratoria met als doel ze te
gebruiken bij de validatie en kwaliteits borging van methoden ingezet bij
residu onderzoek op groeibevorderende stoffen.
For the development of a collection (bank) of reference samples of blank urine 50 different samples of urine were lyophilised in small aliquots. For three species, bovine-, ovine- and porcine-animals samples of urine from 10-20 different animals were collected. The animals differed in race, age, sexes and were fed with different types of feed. After lyophilisation an extensive quality control program was performed. The variability in net weight of the samples of urine and the dry residue after lyophilisation were determined by weighing a percentage of the vials from each batch. The variation in net weight of the samples of urine varied from 0.01% - 1.7%. The variation in net weight of the dry residues varied from 0.1% - 10%. However, most values did not exceed 0.1% for urine and 1% for the dry residues. The residual water after lyophilisation was determined with the Karl-Fisher titration method. The average percentage of water left in the residues varied from 1.0% - 7.0% for samples of bovine urine, from 1.3% - 3.0% for samples of porcine urine and from 1.6% - 5.5% for samples of ovine urine. In 10 out of 50 batches the percentage of residual water exceeded the target value of 5. All samples were analysed for the presence of anabolic compounds with the multi-residue method developed at ARO/CRL. In two samples of bovine urine the presence of a-boldenone was detected and confirmed (1.2 and 1.8 ppb). In most samples of porcine and ovine urine the endogenous a-testosterone and a-estradiol were detected. In several of the samples of porcine and ovine urine a- and b-zeralenol were detected. The sets of reference samples of blank urine are available for official laboratories for the purpose of Quality Assurance of veterinary legislative residue control.
For the development of a collection (bank) of reference samples of blank urine 50 different samples of urine were lyophilised in small aliquots. For three species, bovine-, ovine- and porcine-animals samples of urine from 10-20 different animals were collected. The animals differed in race, age, sexes and were fed with different types of feed. After lyophilisation an extensive quality control program was performed. The variability in net weight of the samples of urine and the dry residue after lyophilisation were determined by weighing a percentage of the vials from each batch. The variation in net weight of the samples of urine varied from 0.01% - 1.7%. The variation in net weight of the dry residues varied from 0.1% - 10%. However, most values did not exceed 0.1% for urine and 1% for the dry residues. The residual water after lyophilisation was determined with the Karl-Fisher titration method. The average percentage of water left in the residues varied from 1.0% - 7.0% for samples of bovine urine, from 1.3% - 3.0% for samples of porcine urine and from 1.6% - 5.5% for samples of ovine urine. In 10 out of 50 batches the percentage of residual water exceeded the target value of 5. All samples were analysed for the presence of anabolic compounds with the multi-residue method developed at ARO/CRL. In two samples of bovine urine the presence of a-boldenone was detected and confirmed (1.2 and 1.8 ppb). In most samples of porcine and ovine urine the endogenous a-testosterone and a-estradiol were detected. In several of the samples of porcine and ovine urine a- and b-zeralenol were detected. The sets of reference samples of blank urine are available for official laboratories for the purpose of Quality Assurance of veterinary legislative residue control.
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