Table S6: Sample preparation, instrumental analysis, validation parameters and application of sent standard mixture for laboratory coded 6
COMPOUND
5-FU
SAMPLE PREP.
Sample preparation
(sample pre-treatment: pH adjustment, filter
pore size, material and trade name,
extraction method and conditions, additional
clean-up, derivatisation, internal
standard,…)
The method is based on on-line Solid-Phase
Extraction (SPE) performed with specific
instrumentation from Spark Holland
(Emmem, The Netherlands).
Filtration of the samples through 0.45 µm
polycarbonate membrane filters.
The pH of the samples is adjusted to 2 with
acetic acid. Concentration by on-line SPE is
carried out with HySphere Resin GP
cartridges (10 x 2 mm ID, from Spark
Holland).
INTRUM. ANALYSIS
Instrumental analysis
(operational parameters: separation
and detection condition,…)
VALIDATION PARAM.
Validation parameters
(sensitivity, accuracy, recovery,
reproducibility,
repeatability,…)
Application of sent mixture
a. Standard mixture was used
for calibration
b. Standard mixture was used
for check-up
c.Standard mixture was not
used
Analysis was performed by LCMS/MS. The separation of the
analytes was performed on a
reversed-phase C18 column. The
detection was performed by using
triple quadrupole MS/MS operating in
the MRM (Multiple Reaction
Monitoring) mode. Ionisation was
carried out by electrospray (ESI) in
the positive mode.
Validation parameters:
b
LOD: 0.1 µg L-1
LOQ: 0.3 µg L-1
Reproducibility: <25 %
Repeatability: <25 %
Recovery: 93%
The determination is controlled by using
isoproturon-d6 as surrogate standard and
tribromophenol and propanil as internal
standard.
CP
The criteria for the recovery of the internal
standards are 70-120%. No internal
standards correction is applied.
The method is based on on-line Solid- The
method is based on on-line Solid-Phase
Extraction (SPE) performed with specific
instrumentation from Spark Holland
(Emmem, The Netherlands).
After on-line SPE, the extracts were
analysed by LC-MS/MS instrument.
The separation of the analytes was
performed on a reversed-phase C18
column. The detection was performed
Validation parameters:
b
Filtration of the samples through 0.45 µm
polycarbonate membrane filters.
The pH of the samples is adjusted to 2 with
acetic acid. Concentration by on-line SPE is
carried out with HySphere Resin GP
cartridges (10 x 2 mm ID, from Spark
Holland).
by using triple quadrupole MS/MS
operating in the MRM (Multiple
Reaction Monitoring) mode. The
ionisation used was electron spray
ionisation (ESI) technique in the
positive mode.
LOD: 0.0012 µg L-1
LOQ: 0.005 µg L-1
Reproducibility: <15 %
Repeatability: <15 %
Recovery: 86 %
ETO
The determination is controlled by using
isoproturon-d6 as surrogate standard and
propanil as internal standard.
The criteria for the recovery of the internal
standards are 70-120%. No internal
standards correction is applied.
The method is based on on-line Solid- The
method is based on on-line Solid-Phase
Extraction (SPE) performed with specific
instrumentation from Spark Holland
(Emmem, The Netherlands).
Filtration of the samples through 0.45 µm
polycarbonate membrane filters.
The pH of the samples is adjusted to 2 with
acetic acid. Concentration by on-line SPE is
carried out with HySphere Resin GP
cartridges (10 x 2 mm ID, from Spark
Holland).
After on-line SPE, the extracts were
analysed by LC-MS/MS instrument.
The separation of the analytes was
performed on a reversed-phase C18
column. The detection was performed
by using triple quadrupole MS/MS
operating in the MRM (Multiple
Reaction Monitoring) mode. The
ionisation used was electron spray
ionisation (ESI) technique in the
positive mode.
Validation parameters:
After on-line SPE, the extracts were
analysed by LC-MS/MS instrument.
Validation parameters:
b
LOD: 0.003 µg L-1
LOQ: 0.01 µg L-1
Reproducibility: <20 %
Repeatability: <20 %
Recovery: 89 %
The determination is controlled by using
isoproturon-d6 as surrogate standard and
propanil as internal standard.
IF
The criteria for the recovery of the internal
standards are 70-120%. No internal
standards correction is applied.
The method is based on on-line Solid- The
method is based on on-line Solid-Phase
Extraction (SPE) performed with specific
b
instrumentation from Spark Holland
(Emmem, The Netherlands).
Filtration of the samples through 0.45 µm
polycarbonate membrane filters.
The pH of the samples is adjusted to 2 with
acetic acid. Concentration by on-line SPE is
carried out with HySphere Resin GP
cartridges (10 x 2 mm ID, from Spark
Holland).
The separation of the analytes was
performed on a reversed-phase C18
column. The detection was performed
by using triple quadrupole MS/MS
operating in the MRM (Multiple
Reaction Monitoring) mode. The
ionisation used was electron spray
ionisation (ESI) technique in the
positive mode.
LOD: 0.0013 µg L-1
LOQ: 0.005 µg L-1
Reproducibility: <10 %
Repeatability: <10 %
Recovery: 84 %
The determination is controlled by using
isoproturon-d6 as surrogate standard and
propanil as internal standard.
MTX
The criteria for the recovery of the internal
standards are 70-120%. No internal
standards correction is applied.
The method is based on on-line Solid- The
method is based on on-line Solid-Phase
Extraction (SPE) performed with specific
instrumentation from Spark Holland
(Emmem, The Netherlands).
Filtration of the samples through 0.45 µm
polycarbonate membrane filters.
The pH of the samples is adjusted to 2 with
acetic acid. Concentration by on-line SPE is
carried out with HySphere Resin GP
cartridges (10 x 2 mm ID, from Spark
Holland).
The determination is controlled by using
isoproturon-d6 as surrogate standard and
propanil as internal standard.
The criteria for the recovery of the internal
standards are 70-120%. No internal
standards correction is applied.
After on-line SPE, the extracts were
analysed by LC-MS/MS instrument.
The separation of the analytes was
performed on a reversed-phase C18
column. The detection was performed
by using triple quadrupole MS/MS
operating in the MRM (Multiple
Reaction Monitoring) mode. The
ionisation used was electron spray
ionisation (ESI) technique in the
positive mode.
Validation parameters:
LOD: 0.05 µg L-1
LOQ: 0.50 µg L-1
Reproducibility: <10 %
Repeatability: <10 %
Recovery: 61%
b