Chinese Journal of Chromatography,
Journal Year:
2023,
Volume and Issue:
41(11), P. 1021 - 1029
Published: Nov. 1, 2023
Organophosphorus
flame
retardants
(OPFRs)
have
emerged
as
good
alternatives
to
brominated
retardants,
the
use
of
which
is
globally
restricted.
In
this
study,
a
screening
method
based
on
QuEChERS-gas
chromatography-quadrupole
time-of-flight
mass
spectrometry
(GC-Q-TOF/MS)
was
established
for
determination
21
OPFRs
in
rice.
First,
full
scan
(scanning
range,
m/z
50-450)
performed
with
mixed
standard
solution
(0.1
μg/g)
by
GC-Q-TOF/MS.
The
fragmentation
pathways
these
were
then
investigated
explore
their
cleavage
fragments,
interrelationships
among
and
possible
modes
alkylated,
chlorinated,
aromatic
OPFRs.
retention
times,
isotopic
abundance
ratios,
molecular
formulas
characteristic
fragments
well
exact
compounds
obtained
establish
spectral
library
Rice
samples
extracted
purified
QuEChERS
method,
0.5%
formate
acetonitrile
used
extraction
solvent;
4
g
magnesium
sulfate,
1
sodium
chloride,
0.5
disodium
hydrogen
citrate,
citrate
extraction-salt
combination;
50
mg
primary
secondary
amine
(PSA),
octadecylsilane
(C18),
150
sulfate
purification
materials.
chromatographic
separation
completed
within
16
min
under
optimized
temperature
program
conditions
DB-5MS
UI
column.
parameters
optimized,
following
conditions:
number
fragment
ions
≥2;
accurate
window=±2×10-5
(±20
ppm);
time
deviation=±0.2
min,
ion
deviation<20%.
developed
applied
samples.
results
indicated
that
matrix
interference
greatly
reduced
decreasing
window,
thereby
improving
signal-to-noise
ratio
analytes.
targets
from
background
noise
using
deconvolution
software,
improved
match
between
target
library.
detection
rates
alkyl
increased
22%
25%,
respectively,
when
spiking
level
2
10
ng/g.
Among
chlorinated
OPFRs,
only
tris(2-chloroisopropyl)
phosphate
(TCIPP)
not
detected
at
ng/g,
indicating
could
be
identified
even
low
concentrations.
matched
those
home-made
well,
practical
application
rice
different
regions
China.
A
total
11
detected,
trimethyl
(TMP),
tri-iso-butyl
(TiBP),
tris(3,5-dimethylphenyl)
(T35DMPP)
had
highest
rates.
These
indicate
three
are
widely
can
easily
come
into
contact
through
various
routes.
Differences
types
actual
may
related
produced
local
factories.
GC-Q-TOF/MS
helpful
identification
complex
Chinese Journal of Chromatography,
Journal Year:
2023,
Volume and Issue:
41(11), P. 1021 - 1029
Published: Nov. 1, 2023
Organophosphorus
flame
retardants
(OPFRs)
have
emerged
as
good
alternatives
to
brominated
retardants,
the
use
of
which
is
globally
restricted.
In
this
study,
a
screening
method
based
on
QuEChERS-gas
chromatography-quadrupole
time-of-flight
mass
spectrometry
(GC-Q-TOF/MS)
was
established
for
determination
21
OPFRs
in
rice.
First,
full
scan
(scanning
range,
m/z
50-450)
performed
with
mixed
standard
solution
(0.1
μg/g)
by
GC-Q-TOF/MS.
The
fragmentation
pathways
these
were
then
investigated
explore
their
cleavage
fragments,
interrelationships
among
and
possible
modes
alkylated,
chlorinated,
aromatic
OPFRs.
retention
times,
isotopic
abundance
ratios,
molecular
formulas
characteristic
fragments
well
exact
compounds
obtained
establish
spectral
library
Rice
samples
extracted
purified
QuEChERS
method,
0.5%
formate
acetonitrile
used
extraction
solvent;
4
g
magnesium
sulfate,
1
sodium
chloride,
0.5
disodium
hydrogen
citrate,
citrate
extraction-salt
combination;
50
mg
primary
secondary
amine
(PSA),
octadecylsilane
(C18),
150
sulfate
purification
materials.
chromatographic
separation
completed
within
16
min
under
optimized
temperature
program
conditions
DB-5MS
UI
column.
parameters
optimized,
following
conditions:
number
fragment
ions
≥2;
accurate
window=±2×10-5
(±20
ppm);
time
deviation=±0.2
min,
ion
deviation<20%.
developed
applied
samples.
results
indicated
that
matrix
interference
greatly
reduced
decreasing
window,
thereby
improving
signal-to-noise
ratio
analytes.
targets
from
background
noise
using
deconvolution
software,
improved
match
between
target
library.
detection
rates
alkyl
increased
22%
25%,
respectively,
when
spiking
level
2
10
ng/g.
Among
chlorinated
OPFRs,
only
tris(2-chloroisopropyl)
phosphate
(TCIPP)
not
detected
at
ng/g,
indicating
could
be
identified
even
low
concentrations.
matched
those
home-made
well,
practical
application
rice
different
regions
China.
A
total
11
detected,
trimethyl
(TMP),
tri-iso-butyl
(TiBP),
tris(3,5-dimethylphenyl)
(T35DMPP)
had
highest
rates.
These
indicate
three
are
widely
can
easily
come
into
contact
through
various
routes.
Differences
types
actual
may
related
produced
local
factories.
GC-Q-TOF/MS
helpful
identification
complex
