quick polar pesticides method

QUICK POLAR PESTICIDES METHOD
PROCEDURE
Quick Polar Pesticides Method
Il metodo QuPPe consente l’analisi dei residui di pesticidi molto polari, non adatti al metodo QuEChERS, sia negli alimenti di origine
vegetale PO (frutta, ortaggi, cereali e prodotti trasformati), sia negli alimenti di origine animale AO (latte e uova).
Il nuovo kit progettato per l’applicazione del metodo QuPPe-PO comprende:
• Analoghi isotopicamente marcati come standards interni (ISTDs);
• Miscele standard di pesticidi polari.
Quick Method for the Analysis of numerous
Highly Polar Pesticides in Foods of Plant Origin via LC-MS/MS
involving Simultaneous Extraction with Methanol (QuPPe-Method)
-
Version 8.1 (March 2015, Document History, see page 58)
Authors: M. Anastassiades; D. I. Kolberg; E. Eichhorn; A. Benkenstein; S. Lukačević;
D. Mack; C. Wildgrube; I. Sigalov; D. Dörk; A. Barth
Note: Changes from V7 to V8 are highlighted in yellow and changes from V8 to 8.1 are highlighted in turquoise
Il nuovo kit progettato per l’applicazione del metodo QuPPe-AO comprende:
• Tubi da centrifuga contenenti ODS (octadecilsilano) come adsorbente;
• Analoghi isotopicamente marcati come standards interni (ISTDs);
• Miscele standard di pesticidi polari.
PRODOTTI DI ORIGINE ANIMALE
Pesare una quantità rappresentativa di campione
omogeneizzato in un tubo da centrifuga di 50 ml
Pesare una quantità rappresentativa di campione
omogeneizzato in un tubo da centrifuga di 50 ml
Frutta fresca, verdura e succhi di frutta: 10 g ± 0,1 g
Frutta secca e funghi secchi: 5 g ± 0,05 g oppure 13,5 g ± 0,1 g di campione
reidratato ed omogeneizzato (corrispondente a 5 g di campione secco)
Cereali, legumi secchi e miele: 5 g ± 0,05 g
Aggiungere acqua fino ad un contenuto totale di circa
10 g a seconda della natura della matrice (Tabella 19)
Content
1
Scope and Short Description
2
2
Apparatus and Consumables
2
3
Chemicals
4
4
Disclaimer
5.6.2
Method 1.1
“Glyphosate
& Co. AS 11”
Authors:
M. Anastassiades;
D. I. Kolberg; D. Mack; A. Barth; Chr. Wildgrube; D. Roux
- Version
1 (Mar 2013, Document History, see page 15)
Method 1.2 “Glyphosate
& Co. AS 11-HC”
Quick Method for the Analysis of Residues of numerous 6
Quick
for the
Analysis
of Residues
of numerous
5 Highly
7
Procedure
PolarMethod
Pesticides
in Food
Commodities
involving
Simultane5.1
7
Highly
Polar
Pesticides
in Food
Commodities
involving
SimultaneSample
preparation
Quick
Method
forMethanol
the
Analysis
of Residues
of via
numerous
ous
Extraction
with
and
Determination
LC-MS/MS
5.2
7
Extraction
/ Centrifugation
/ Filtration
ous
Extraction
with
Methanol
and
Determination
via LC-MS/MS
Highly
Polar
Pesticides
in
Food
Commodities
involving
Simultane(QuPPe-AO-Method)
Quick
5.3
9
Blank
extractsMethod for the Analysis of Residues of numerous
(QuPPe-AO-Method)
ous Extraction
with Methanol
Determination
via LC-MS/MS
Highly
Polar
Pesticides
in Food and
Commodities
involving
Simultane5.4
9
Recovery
experiments
(QuPPe-AO-Method)
5.5 ous
9
II.
Food
of
Animal
Origin
Preparation
of
calibration
standards
Extraction with Methanol and Determination via LC-MS/MS
II.
Food
of
Animal
Origin
5.6
12
LC-MS/MS Measurement
(QuPPe-AO-Method)
Version
1
(Mar
2013,
Document
History,
see
page
15)
5.6.1
13
II.1Food
ofused
Animal
Origin
Practical Information: Methods currently
routinely
at CVUA Stuttgart
Authors:- M.Version
Anastassiades;
D. 2013,
I. Kolberg;
D. Mack; History,
A. Barth; Chr.
(Mar
Document
see Wildgrube;
page 15)D. Roux
5.6.3
5.6.4
1.
II. Food of Animal Origin
Authors: M. Anastassiades; D. I. Kolberg; D. Mack; A. Barth; Chr. Wildgrube; D. Roux
14
17
20
Methodand
1.3 “Glyphosate
&
Co. Hypercarb”
Scope
Short
Description
- Version
1 (Mar 2013, Document History, see page 15)
Scope
Short
Description
28
Methodand
1.4
“PerChloPhos”
Authors:
M. Anastassiades;
D. I. Kolberg; D. Mack; A. Barth; Chr. Wildgrube; D. Roux
A method
is described
forMaleic
the residue
analysis of very polar, non-QuEChERS-amenable, pesticides
5.6.6
29
Method
2 “Fosetyl
and
Hydrazide”
1. Scope
and
Short
Description
A method is described for the residue analysis of very polar, non-QuEChERS-amenable, pesticides
1.
5.6.5
in
in
of animal
This
first
31 will
Method 3origin.
“Amitrole
& Co.
” version of the method was tested for milk and eggs. More commodities
food
of animal
origin.Short
This
version
the method
was polar,
testednon-QuEChERS-amenable,
for milk and eggs. More commodities
A method
is described
forfirst
the
residueofanalysis
of very
pesticideswill
in
1.
Scope
and
Description
food
5.6.7
5.6.8
gradually
follow.
Method
4.1 “Quats & Co. Obelisc R”
33
gradually
follow.
food of animal
origin. This first version of the method was tested for milk and eggs. More commodities will
5.6.9
Method
4.2adjustment
“Quats &for
Co.the
BEH-Amide
” analysis
Following
water
and
addition
of acidified
methanol
are extracted from thepesticides
test 35
portion
A method
is described
residue
of very
polar,residues
non-QuEChERS-amenable,
in
Following
water
adjustment
and addition
of acidified methanol residues are extracted from the test 37
portion
gradually
follow.
5.6.10
Method
5origin.
“Quats
&centrifugation,
Co.first
MonoChrom
via
Following
an
of thewas
rawtested
extract
cleaned-up
byMore
simultaneous
dilution
foodshaking.
of animal
This
versionMS”
of aliquot
the method
forismilk
and eggs.
commodities
will
5.6.11
38
Method
6 “Streptomycin
and
via
shaking.
Following
centrifugation,
an of
aliquot
of the
raw extract
is cleaned-up
by simultaneous
Following
water
adjustment
andKasugamycin
addition
acidified
methanol
residues
are extracted
from the test dilution
portion
with
acetonitrile
gradually
follow. and dSPE with ODS sorbent, which leads to a precipitation or adsorption of a large por39 porto a precipitation
or adsorption
of a large
extract
is cleaned-up
by simultaneous
dilution
5.6.12
Method
7 “Morpholine,
Diethanolamine
Triethanolamine
with
acetonitrile
and dSPE
with ODS sorbent,
which
via shaking.
Following
centrifugation,
anand
aliquot
of theleads
raw
Following
water
adjustment
and addition
of acidified
methanol
residues
from the
portion
tion of co-extractives.
The cleaned-up
extract
is centrifuged
and
filteredare
andextracted
then subjected
to test
determina5.6.13
40
Method
8 “TDMs
with
acetonitrile
and dSPE
with ODS sorbent,
leads toand
a precipitation
or adsorption
large portion of
co-extractives.
The cleaned-up
extract iswhich
centrifuged
filtered and then
subjectedoftoadetermina-
via
Following
centrifugation,
an aliquot ofmethods
the rawfor
extract
is cleaned-upanalysis
by simultaneous
dilution
tive shaking.
analysis
via LC-MS/MS.
Various LC-MS/MS
the simultaneous
of different
5.7
41comCalibration
and Calculations
tive
via LC-MS/MS.
Various LC-MS/MS
methods forand
thefiltered
simultaneous
of different
tion analysis
of co-extractives.
The cleaned-up
extract is centrifuged
and thenanalysis
subjected
to determina6binations
45comPerformance
Data
with acetonitrile
and
dSPE
with ODSQuantification
sorbent, which
leads
a precipitation
adsorption
large
porof pesticides
are provided.
is in
mosttocases
performedorwith
the helpofofaisotopically
of pesticides
are provided.
is in most
performed with
the help
of isotopically
tive analysis
via LC-MS/MS.
VariousQuantification
LC-MS/MS methods
forcases
the simultaneous
analysis
of different
7binations
46comReferences
labeled
analogues of the
analytes,
which
used asand
internal
standards
(ISTDs).
So to
fardeterminaavailable,
tion of co-extractives.
Thetarget
cleaned-up
extract
is are
centrifuged
filtered
and then
subjected
labeled
of the
analytes,
which areisused
as internal
standardswith
(ISTDs).
So of
farisotopically
available,
binationsanalogues
of pesticides
aretarget
provided.
Quantification
in most
cases performed
the help
these
ISTDs are
added directly
to the LC-MS/MS
test portion methods
at the beginning
of the procedure
to compensate
forcomany
tive analysis
via LC-MS/MS.
Various
for the simultaneous
analysis
of different
these
are added
directly
the test which
portionare
at the
beginning
of the
procedure
to compensate
for any
labeledISTDs
analogues
of the
target to
analytes,
used
as internal
standards
(ISTDs).
So far available,
factors
having
an influence
on the recovery-rates
such
volume-deviations,
losses
extracbinations
of pesticides
are provided.
Quantification
is inas
most
cases performedanalyte
with the
help during
of isotopically
factors
havingare
anadded
influence
on the
recovery-rates
volume-deviations,
analytetolosses
during for
extracthese ISTDs
directly
to the
test portion such
at theasbeginning
of the procedure
compensate
any
tion andanalogues
cleanup asofwell
matrix-effects
LC-MS/MS.
labeled
theas
target
analytes, during
which are
used as internal standards (ISTDs). So far available,
tion andhaving
cleanup
well as on
matrix-effects
during LC-MS/MS.
factors
anas
influence
the recovery-rates
such as volume-deviations, analyte losses during extracthese ISTDs are added directly to the test portion at the beginning of the procedure to compensate for any
tion and cleanup as well as matrix-effects during LC-MS/MS.
EU
Reference
foron
pesticides
requiring Single
Residue
Methods (EURL-SRM)
1 of 60
factors
havingLaboratory
an influence
the recovery-rates
such as
volume-deviations,
analyte losses during
extrac-
2. Apparatus
and3/2,
Consumables
CVUA
Stuttgart, Schaflandstr.
DE-70736 Fellbach, Germany
tion
cleanup asand
well as
matrix-effects
during LC-MS/MS.
Website:
www.eurl-pesticides.eu,
E-Mail:
[email protected]
2. and
Apparatus
Consumables
2.1. Powerful sample homogenizer,
e.g. Braun MR 5550 hand blender (with chopper attachment)
2.
Apparatus
and
e.g.2.1.
Braun
MR 5550sample
handConsumables
blender
(with chopper attachment)
Powerful
homogenizer,
Economicamente
vantaggiosi:
consegna periodica
di lotti sempre
freschi
Aggiungere 10 ml di metanolo acidificato (CH3OH + 1% F.A.)
e 50 μl di IS (IS-working solution I) contenente gli analoghi
isotopicamente marcati di uno o più analiti d’interesse
Agitare vigorosamente mediante un agitatore meccanico
tipo Vortex (Prodotti freschi: 5-15 min; Prodotti secchi:
15-30 min) oppure, in alternativa, agitare manualmente per
1 min quindi, nel solo caso di prodotti secchi, agitare per un
altro minuto dopo un “soaking period” di 15-30 min
Per determinare il Paraquat ed il Diquat dopo la prima agitazione manuale della
durata di 1 min, effettuare un trattamento termico di 15 min in un bagno ad
acqua a 80°C. In seguito, agitare nuovamente per 1 min e
condizionare il campione a temperatura ambiente
Centrifugare
per 5 min a 4000 rpm
Powerful sample
homogenizer,
2. 2.1.
Apparatus
and Consumables
Ready to use
Standards:
manipolazione ed
impiego più sicuri
PRODOTTI DI ORIGINE VEGETALE
e.g. Braun MR 5550 hand blender (with chopper attachment)
Aggiungere acqua fino ad un contenuto totale di circa 10 g.
Aggiungere 1,2 g di acqua nel caso di latte vaccino (88%
H2O) e 2,4 g di acqua nel caso di uova di pollo (76% H2O)
Aggiungere 10 ml di metanolo acidificato (CH3OH + 1% F.A.)
e 50 μl di IS (IS-working solution I) contenente gli analoghi
isotopicamente marcati di uno o più analiti d’interesse
Agitare vigorosamente mediante un agitatore meccanico
tipo Vortex per 5-20 min oppure, in alternativa,
agitare manualmente per 1 min
Centrifugare
per 5 min a >3000 g
Trasferire un’aliquota (2 ml) in un tubo di 10 ml, contenente
100 mg di ODS come adsorbente (Codice: QPPAO01)
e 2 ml di acetonitrile
Agitare manualmente
per 1 min
2.1. Powerful sample homogenizer,
e.g. Braun MR 5550 hand blender (with chopper attachment)
EU Reference Laboratory for pesticides requiring Single Residue Methods (EURL-SRM)
CVUA
Stuttgart, Schaflandstr.
DE-70736 Fellbach,
Germany
EU Reference
Laboratory 3/2,
for pesticides
requiring
Single Residue Methods (EURL-SRM)
Website:
www.eurl-pesticides.eu,
[email protected]
CVUA Stuttgart,
Schaflandstr. 3/2,E-Mail:
DE-70736
Fellbach, Germany
EU
Reference
Laboratory forE-Mail:
pesticides
requiring Single Residue Methods (EURL-SRM)
Website:
www.eurl-pesticides.eu,
[email protected]
CVUA Stuttgart, Schaflandstr. 3/2, DE-70736 Fellbach, Germany
Website: www.eurl-pesticides.eu, E-Mail: [email protected]
EU Reference Laboratory for pesticides requiring Single Residue Methods (EURL-SRM)
CVUA Stuttgart, Schaflandstr. 3/2, DE-70736 Fellbach, Germany
Website: www.eurl-pesticides.eu, E-Mail: [email protected]
1 of 15
1 of 15
1 of 15
1 of 15
Filtrare un’aliquota (3 ml) di estratto in
un contenitore di stoccaggio richiudibile
Usare contenitori in plastica nel caso di pesticidi
(Paraquat, Diquat, Streptomycin, Glyphosate, etc.)
che tendono ad interagire con le superfici dei
contenitori in vetro
Trasferire una o più aliquote (1 ml)
di estratto filtrato in vials per analisi LC
Quantificazione
più accurata:
analoghi
isotopicamente
marcati
Latte fresco e uova fresche: 10 g ± 0,05 g
Valutazione
dei fenomeni di
interazione con
i contenitori
Centrifugare
per 5 min a >3000 g
Filtrare un’aliquota (circa 3-4 ml) di estratto purificato
in un contenitore di stoccaggio richiudibile
Trasferire una o più aliquote (1 ml)
di estratto filtrato in vials per analisi LC
Metodo: QuPPe-AO V14 g MgSO₄, 1 g NaCl, 1 g SCTD, 0,5
0,1 g ODS
Confezionamento
50 Tubi (10 ml)
Codice
QPPAO01
STANDARD MIX 1.1
Confezionamento
1 x 1,1 ml fiala silanizzata ambrata
Analiti
Ethephon
HEPA
CAS
16672-87-0
22987-21-9
STANDARD MIX 4.1
Confezionamento
Solvente
Concentrazione
Codice
Metanolo
5 mg/l
CRM3G11L344
Analiti
Glyphosate
AMPA
CAS
1071-83-6
1066-51-9
Analiti
Glufosinate
MPPA
CAS
51276-47-2
15090-23-0
Analiti
N-Acetyl Glufosinate
CAS
73634-73-8
1 x 1,1 ml fiala silanizzata ambrata
Analiti
Diquat
Paraquat
Chlormequat
CAS
2764-72-9
4685-14-7
7003-89-6
Solvente
Concentrazione
Codice
Metanolo
5 mg/l
CRM3G11L350
Analiti
CAS
15302-91-7
Mepiquat
1596-84-5
Daminozide
57-14-7
N,N-Dimethylhydrazine
STANDARD MIX 1.2
Confezionamento
1 x 1,1 ml fiala silanizzata ambrata
Analiti
Ethephon
HEPA
Glyphosate
CAS
16672-87-0
22987-21-9
1071-83-6
Concentrazione
Codice
Metanolo
5 mg/l
CRM3G11L345
CAS
1066-51-9
51276-47-2
15090-23-0
Analiti
N-Acetyl Glufosinate
Fosetyl-Aluminium
N-Acetyl AMPA
CAS
73634-73-8
39148-24-8
57637-97-5
Analiti
Phosphonic acid
CAS
66215-27-8
2181-42-2
1631-58-9
Analiti
Difenzoquat
Melamine
Propamocarb
CAS
49866-87-7
108-78-1
24579-73-5
STANDARD MIX 4.2
Solvente
Analiti
AMPA
Glufosinate
MPPA
Analiti
Cyromazine
Trimethylsulfonium
Nereistoxin
CAS
13598-36-2
Confezionamento
1 x 1,1 ml fiala silanizzata ambrata
Analiti
Amitrole
ETU
Chlormequat
Mepiquat
CAS
61-82-5
96-45-7
7003-89-6
15302-91-7
Solvente
Concentrazione
Codice
Metanolo
5 mg/l
CRM3G11L351
Analiti
Daminozide
PTU
Cyromazine
Trimethylsulfonium
CAS
1596-84-5
2122-19-2
66215-27-8
2181-42-2
Analiti
Nereistoxin
Difenzoquat
Melamine
Propamocarb
CAS
1631-58-9
49866-87-7
108-78-1
24579-73-5
Analiti
Morpholine
Diethanolamine
Triethanolamine
CAS
110-91-8
111-42-2
102-71-6
STANDARD MIX 1.3
Confezionamento
1 x 1,1 ml fiala silanizzata ambrata
Analiti
Ethephon
HEPA
Glyphosate
AMPA
CAS
16672-87-0
22987-21-9
1071-83-6
1066-51-9
STANDARD MIX 5
Solvente
Concentrazione
Codice
Metanolo
5 mg/l
CRM3G11L346
Analiti
N-Acetyl AMPA
Glufosinate
MPPA
N-Acetyl Glufosinate
CAS
57637-97-5
51276-47-2
15090-23-0
73634-73-8
Analiti
Fosetyl-Aluminium
Phosphonic acid
Maleic hydrazide
Perchlorate
CAS
39148-24-8
13598-36-2
10071-13-3
14797-73-0
Analiti
Chlorate
Cyanuric acid
Bialaphos
CAS
14866-68-3
108-80-5
35597-43-4
Confezionamento
1 x 1,1 ml fiala silanizzata ambrata
Analiti
Chlormequat
Mepiquat
CAS
7003-89-6
15302-91-7
Solvente
Concentrazione
Codice
Metanolo
5 mg/l
CRM3G11L352
Analiti
Difenzoquat
ETU
CAS
49866-87-7
96-45-7
1 x 1,1 ml fiala silanizzata ambrata
Analiti
Phosphonic acid
CAS
13598-36-2
Analiti
Perchlorate
Solvente
Concentrazione
Codice
Metanolo
5 mg/l
CRM3G11L347
CAS
14797-73-0
Analiti
Chlorate
Confezionamento
1 x 1,1 ml fiala silanizzata ambrata
Analiti
Streptomycin
CAS
14866-68-3
CAS
57-92-1
Solvente
Concentrazione
Codice
Metanolo
5 mg/l
CRM3G11L353
Analiti
CAS
Kasugamycin
6980-18-3
STANDARD MIX 2
Confezionamento
1 x 1,1 ml fiala silanizzata ambrata
Analiti
Fosetyl-Aluminium
CAS
39148-24-8
Analiti
Maleic hydrazide
STANDARD MIX 7
Solvente
Concentrazione
Codice
Metanolo
5 mg/l
CRM3G11L348
CAS
10071-13-3
Analiti
Perchlorate
CAS
14797-73-0
Confezionamento
1 x 1,1 ml fiala silanizzata ambrata
Analiti
Morpholine
CAS
110-91-8
Solvente
Concentrazione
Codice
Metanolo
5 mg/l
CRM3G11L354
Analiti
Diethanolamine
CAS
111-42-2
1 x 1,1 ml fiala silanizzata ambrata
Analiti
Amitrole
Chlormequat
Mepiquat
CAS
61-82-5
7003-89-6
15302-91-7
Analiti
Daminozide
ETU
PTU
Solvente
Concentrazione
Codice
Metanolo
5 mg/l
CRM3G11L349
CAS
1596-84-5
96-45-7
2122-19-2
Analiti
Trimethylsulfonium
Difenzoquat
Cyromazine
Analiti
Triethanolamine
CAS
102-71-6
STANDARD MIX 8
STANDARD MIX 3
Confezionamento
CAS
2122-19-2
STANDARD MIX 6
STANDARD MIX 1.4
Confezionamento
Analiti
PTU
CAS
2181-42-2
49866-87-7
66215-27-8
Confezionamento
Solvente
1 x 1,1 ml fiala silanizzata ambrata
Analiti
1,2,4-Triazole
Triazole-alanine
CAS
288-88-0
86362-20-1
Analiti
Triazole-acetic acid
Triazole-lactic acid
Acqua
CAS
28711-29-7
N.D.
Concentrazione
Codice
5 mg/l
CRM3J11L355
Analiti
1,2,3-Triazole
sito web/e-commerce www.labinstruments.org
CAS
288-36-8
e-mail [email protected]
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