cis-DCCA
(0.015;
0.020); DF, 97%
trans-DCCA
(0.015; 0.030);
DF, 100%
DBCA (0.015;
0.025); DF, 97%
3PBA (0.015;
0.025); DF, 100%
4F3PBA (0.015;
0.025); DF, 10%
V: 5 mL
H: Enzymatic
E: LLE
C: LLE
I: LC-MS/MS (triple quadrupole;
negative mode)
LLE:
• Extraction: 2
 6 mL hexane
• Re-extraction to 3 mL 0.1 M NaOH
• Re-extraction to 0.2 mL conc.
HCl + 6 mL hexane
• Evaporation
– gentle stream of
nitrogen
• Reconstitution in 80
μL 0.1% formic
acid in water/methanol mixture (70/30,
v/v)
• Extraction similar to Schettgen et al.
[11]
• Population: 39 adults
– 23 women and
16 men
– aged between 24 and 62 years old
Limousin Region, France
[14]
4F3PBA (0.019;
nd); DF, 54%
3PBA (0.018; nd);
DF, 82%
V: 1 mL
H: enzymatic
E: SPE (Oasis HLB 3 cc, waters)
C: No
I: UPLC-MS/MS (triple quadrupole, ESI-)
SPE:
• Conditioning: 1 mL MeOH/acetone
(25:75); 1 mL 1% CH
3 COOH in water
• Sample
• Washing: 0.5 mL 1% CH
3 COOH in
water
• Cartridge drying (20 min under
vacuum)
• Elution: 1.5 mL MeOH/acetone
(25:75)
• Evaporation
– gentle stream of
nitrogen
• Reconstitution in 120
μL MeOH:
H
2 O (25:75)
• External quality control: G-EQUAS
• Population: human urine samples from
two adult Spanish populations in Catalonia
and Galicia (n
¼ 125), Spain
[21]
cis-DBCA
(0.1;
nd); DF, nd
cis-DCCA
(0.2;
nd); DF, nd
trans-DCCA
(0.4;
nd); DF, nd
4F3PBA (0.2; nd);
V: 2 mL
H: enzymatic
E: SPE (Oasis HLB 3 cc, waters)
C: No
I: HPLC-TIS-MS/MS (triple
quadrupole, negative mode)
SPE:
• Conditioning: 1 mL MeOH, 1 mL 1%
CH
3 COOH in water
• Sample
• Washing: 5% MeOH in 1% acetic
acid solution
• Cartridge drying (30 s
– vacuum)
• Population: 115 samples
[30]
(continued)
Analytical Methods for Determination Urinary Metabolites of Synthetic. . .
69