Progetto Trieste 2011, 1st round, Veterinary Drug Residues
Proficiency Testing Service by Test Veritas S.r.l.
TEST MATERIAL: U1111-1A and U1111-2A (confirmatory)
RAL’s IN BOVINE URINE - incurred
2011, 1st round
Test material A are two different samples: 1A and 2A - please test both materials!
LABORATORY: …
ANALYST: ...
COMPOUNDS
U1111-1A
RESULTS
CONCENTRATION
CORRECTED FOR
RECOVERY*
(g/l)
RECOVERY
%
DATE: ...
SPECIFICATIONS
DECISION
DETECTION
LIMIT
ISO
CAPABILITY
17025**
CC or
CC
cut-off
yes/no
(g/l)
(g/l)
ZERANOL
TALERANOL
COMPOUNDS
U1111-2A
RESULTS
CONCENTRATION
CORRECTED FOR
RECOVERY*
(g/l)
RECOVERY
%
SPECIFICATIONS
DECISION
DETECTION
LIMIT
ISO
CAPABILITY
CC or
17025**
CC
cut-off
yes/no
(g/l)
(g/l)
ZERANOL
TALERANOL
Please indicate the concentration in relation to liquid urine sample (not of the powder)
Comments:
* Please indicate:
 estimated concentration corrected with recovery if the compound is detected;
 "< of…" if the compound is not detected;
 "NS" if the compound is not searched (see example above reported).
**Please indicate whether the method used is in the scope of accreditation (choose “yes” if the methods is
already accreditated).
Example:
COMPOUNDS
Compound 1
Compound 2
Compound 3
RESULTS
SPECIFICATIONS
CONCENTRATION
CORRECTED FOR
RECOVERY*
(g/l)
RECOVERY
%
3.2
NS
< 0.5
80
-
DECISION
LIMIT
CC or
cut-off
(g/l)
1.0
0.5
DETECTION
CAPABILITY
CC
(g/l)
ISO
17025**
yes/no
1.5
1.0
y
n
TEST MATERIAL: U1111-1A and U1111-2A (confirmatory)
PAGINA 1 di 5
REVISIONE
DATA DELLA REVISIONE
N. 0
03/01/2011
The data of your analyses will be preserved for 5 years and then will be destroyed.
D:\106745372.doc
DOCUMENTO AGGIORNATO IL 01/03/11
Progetto Trieste 2011, 1st round, Veterinary Drug Residues
Proficiency Testing Service by Test Veritas S.r.l.
RAL’s IN BOVINE URINE - incurred
2011, 1st round
LABORATORY: …
ANALYST: …
MARK YOUR CHOICE
Analytical methods used by participants
Methods
GC/MS
GC/MS/MS
Other (specify)
HPLC/MS
HPLC/MS/MS
UPLC/MS/MS
Is the analytical method a routine one?
No
Yes
Source of standards for chromatographyc analysis
ZER
TAL
Sigma, Aldrich, Fluka
Riedel-de Haen
RIVM
Steraloids
NARL
dr. Ehrenstorfer
Other (specify)
Sample preparation
Amount of test sample for the extraction
Sample volume (ml)
5
10
Other (specify)
1.5
2
3
Sample treatment
C18
C18 + NH2
Liq-Liq extraction (n-hexan)
Liq-Liq extraction (dichloromethane)
Liq-Liq extraction (TBME)
Liq-Liq extraction (ether)
-glucoronidase
-gluc-aryl sulfatase
Extraction (SPE or other)
SPE extraction
OASIS® HLB
Other (specify)
Other extraction
pentane
„Detectabuse® “ column
Other (specify)
Digestion
Other (specify)
TEST MATERIAL: U1111-1A and U1111-2A (confirmatory)
RAL’s IN BOVINE URINE - incurred
PAGINA 2 di 5
REVISIONE
DATA DELLA REVISIONE
N. 0
03/01/2011
The data of your analyses will be preserved for 5 years and then will be destroyed.
D:\106745372.doc
DOCUMENTO AGGIORNATO IL 01/03/11
Progetto Trieste 2011, 1st round, Veterinary Drug Residues
Proficiency Testing Service by Test Veritas S.r.l.
2011, 1st round
LABORATORY: …
C18
C18+ NH2
OASIS®
OASIS® HLB
Immunoaffinity chromatography
Liq-Liq extraction (TBME)
Liq-Liq extraction (n-hexane)
ANALYST: …
Clean up (SPE or other)
SPE clean up
Nexus + NH2
Strata® - X
Envi Chrom P+NH2+SiOH
Other (specify)
Other clean up
Liq-Liq extraction (ether)
Liq-Liq extraction (diethyl ether)
Other (specify)
HPLC methodology and conditions
HPLC
Isocratic
Column phase
Other (specify)
Column length (cm)
15
Other (specify)
Column diameter (mm)
3
Other (specify)
Particle size (m)
3.5
5
Other (specify)
Cromatographyc column (type)
Prodigy®
Symmetry®
Synergi®
Superspher®
SupelcosilTM
Ultrabase®
X-BridgeTM
X-terra®
YMCTM
Zebron®
Zorbax®
Other (specify)
Gradient
C18
5
10
2
2.1
1.7
2.5
3
AcquityTM
AscentisTM
AtlantisTM
Beckman
Betasil
GeminiTM
Hypersil®
Hypercab®
HyPURITY
Lichrospher®
Luna®
Novapak®
Nucleodur®
water / methanol
water / acetonitrile
water / methanol / acetonitrile
acetonitrile / water / acetic acid
acetic acid / acetonitrile
Mobil phase
formic acid / acetonitrile
formic acid / water / acetonitrile
ammonium / water / acetonitrile
ammonium acetate / methanol
Other (specify)
TEST MATERIAL: U1111-1A and U1111-2A (confirmatory)
RAL’s IN BOVINE URINE - incurred
2011, 1st round
PAGINA 3 di 5
REVISIONE
DATA DELLA REVISIONE
N. 0
03/01/2011
The data of your analyses will be preserved for 5 years and then will be destroyed.
D:\106745372.doc
DOCUMENTO AGGIORNATO IL 01/03/11
Progetto Trieste 2011, 1st round, Veterinary Drug Residues
Proficiency Testing Service by Test Veritas S.r.l.
LABORATORY: …
x<5
5<x<6
6 < x < 6.5
x < 0.2
0.2 < x < 0.3
0.3 < x < 0.4
ANALYST: …
HPLC
pH of mobile phase
6.5 < x < 7
x>7
Other (specify)
Flow rate (ml/min)
0.4 < x < 0.5
x > 0.5
Other (specify)
Post column reagent
... (specify)
5 < x < 10
10 < x < 20
20 < x < 30
Injection volume (l)
30 < x < 40
40 < x < 50
Other (specify)
UV(nm)
… (specify)
GC methodology
GC
Capillary column length (m)
Other (specify)
25
30
0.25
CP-SIL 8 CB/MS
DB-1MS
DB-5MS
HP-5MS
J&W
1
2
240
250
Splitless
Pulsed splitless
80-300
80-320
95-295
Film thickness (m)
Other (specify)
Cromatographyc column
Perking Elmer Elite 5MS
OPTIMA-5-MS
WCOT Fused silica
Zebron® ZB-1
Other (specify)
Injection volume (l)
4
Other (specify)
Injection temperature (°C)
280
Other (specify)
Injection procedure
Split
Other (specify)
Oven temperature (°C)
120-130
120-300
Other (specify)
TEST MATERIAL: U1111-1A and U1111-2A (confirmatory)
RAL’s IN BOVINE URINE - incurred
2011, 1st round
PAGINA 4 di 5
REVISIONE
DATA DELLA REVISIONE
N. 0
03/01/2011
The data of your analyses will be preserved for 5 years and then will be destroyed.
D:\106745372.doc
DOCUMENTO AGGIORNATO IL 01/03/11
Progetto Trieste 2011, 1st round, Veterinary Drug Residues
Proficiency Testing Service by Test Veritas S.r.l.
LABORATORY: …
ANALYST: …
Number of replicates (1 replicates = 1 extracion)
1
2
Number of extraction
Other (specify)
Recovery (HPLC and GC)
Internal standard
Spiked sample
In-house Reference Material (RM)
Recovery calculated by
Matrix matched calibration
Other (specify)
Quality (HPLC and GC)
Quality control implemented
Control chart with in-house
Reference Material (RM)
Control chart with Certified
Reference Material (CRM)
Regular partecipation to
proficency test (PT)
Blank sample
Duplicate analyses
Spiked sample
Other (specify)
Reference (HPLC and GC)
Internal method
PAGINA 5 di 5
Reference
Other (specify)
REVISIONE
DATA DELLA REVISIONE
N. 0
03/01/2011
The data of your analyses will be preserved for 5 years and then will be destroyed.
D:\106745372.doc
DOCUMENTO AGGIORNATO IL 01/03/11