DCCA (mixture of
isomers) (0.02; nd);
DF, 100%
DBCA (0.04; nd); DF,
50%
3PBA (0.06; nd); DF,
100%
4F3PBA (0.02; nd);
DF, 100%
MPA (0.04; nd); DF,
0%
CPBA (0.04; nd);
DF,70%
ClF3CA (0.08, nd);
DF, 80%
V: 2.5 mL
H: enzymatic
E: automatic SPE (C18
Agilent SampliQ, 200 mg)
C: No
I: GC-MS (quadrupole, EI,
SIM)
SPE:
• Conditioning: 6 mL MeOH,
3 mL ACN, 3 mL 2% HCOOH
• Sample
• Washing: 1.5 mL 20%
MeOH 2% HCOOH in water
• Drying
• Elution: 3.5 mL ACN
• Concentration to 200
μL
(TurboVap Evaporator)
• Derivatization
• LLE: 200
μL isooctane
• 20
μL DIC, 30
μL HFIP
(vortexing 10 min)
• Wash: 1 mL 1 M NaHCO
3
• SPE (C18)
–
RapidTrace auto-SPE
WorkStation;
• Population: ten
children living in
Boston, MA (USA)
[33]
Analytical Methods for Determination Urinary Metabolites of Synthetic. . .
67
isomers) (0.02; nd);
DF, 100%
DBCA (0.04; nd); DF,
50%
3PBA (0.06; nd); DF,
100%
4F3PBA (0.02; nd);
DF, 100%
MPA (0.04; nd); DF,
0%
CPBA (0.04; nd);
DF,70%
ClF3CA (0.08, nd);
DF, 80%
V: 2.5 mL
H: enzymatic
E: automatic SPE (C18
Agilent SampliQ, 200 mg)
C: No
I: GC-MS (quadrupole, EI,
SIM)
SPE:
• Conditioning: 6 mL MeOH,
3 mL ACN, 3 mL 2% HCOOH
• Sample
• Washing: 1.5 mL 20%
MeOH 2% HCOOH in water
• Drying
• Elution: 3.5 mL ACN
• Concentration to 200
μL
(TurboVap Evaporator)
• Derivatization
• LLE: 200
μL isooctane
• 20
μL DIC, 30
μL HFIP
(vortexing 10 min)
• Wash: 1 mL 1 M NaHCO
3
• SPE (C18)
–
RapidTrace auto-SPE
WorkStation;
• Population: ten
children living in
Boston, MA (USA)
[33]
Analytical Methods for Determination Urinary Metabolites of Synthetic. . .
67
