• Washing: 5 mL hexane and
2 mL hexane-toluene (70:30)
• Elution: 8 mL hexane-toluene
(60:40)
• Evaporation
– gentle stream
of nitrogen
• Reconstitution: 0.5 mL
hexane
CDCA (0.0088;
0.029); DF, 52.6–
69.4%
cis-DCCA
(0.0072;
0.024); DF, 95.6–
95.9%
trans-DCCA
(0.0096;
0.032); DF, 94.7–
100%
DBCA (0.0060;
0.020); DF, 5.3–
12.2%
3PBA (0.013; 0.043);
DF, 91.8–94.7%
4F3PBA (0.0053;
0.018); DF, 32.5–
55.1%
V: 5 mL
H: enzymatic
E: LLE
I: GC-MS (quadrupole,
SIM, negative mode)
LLE:
• Extraction: 2
 5 mL DCM
• Evaporation
• 250
μL ACN, 30
μL HFIP,
20
μL DIIC, 10 min, RT
• Wash and extraction: 1 mL
1 M NaHCO
3 + 250
μL hexane
• External Quality
Control: G-EQUAS
• Population: rural
population of the
Montérégie area,
Quebec (adults
n
¼ 114, children,
n
¼ 49), Canada
[25]
cis-DCCA
(0.007;
nd); DF, 99%
trans-DCCA
(0.01;
nd); DF, 99%
DBCA (0.006; nd);
DF, 77%
3PBA (0.01; nd); DF,
100%
4F3PBA (0.008; nd);
DF, 71%
V: 5 mL
H: enzymatic
E: LLE
C: No
I: GC-MS (quadrupole,
negative mode, SIM)
LLE:
• Extraction: 9 mL n-hexane
• Evaporation to dryness
• 30
μL HFIP, 20
μL DIIC,
2 mL of iso-octane/hexane (2:98)
• Evaporation
• Reconstitution: hexane
• External quality
control: (G-EQUAS)
• Population: pregnant women residing
in ten Englishspeaking Caribbean
countries (n
¼ 295)
[22]
(continued)
Analytical Methods for Determination Urinary Metabolites of Synthetic. . .
61