Table 2
(continued)
Analytes (LOD
ng/mL; LOQ ng/mL);
DF
Sample volume (V),
hydrolysis (H), extraction
(E), cleanup (C),
instrument (I)
Extraction and cleanup details
Derivatization
Notice
Ref.
of saturated NaCl + 2
 5 mL
n-hexane
• Evaporation to dryness (gentle stream of nitrogen)
• Reconstitution: 1 mL hexane
cis-DCCA
(0.5; nd);
DF, 100%
trans-DCCA
(0.5;
nd); DF, 100%
DBCA (0.3; nd); DF,
nd
3PBA (0.5; nd); DF,
100%
4F3PBA (0.5; nd);
DF, nd
V: 10 mL
H: acidic (2 mL H
2 SO
4 ;
1 h, 90
C)
E: SPE (C18, 500 mg,
Bakerbond)
I: GC-MS (quadrupole,
SIM)
SPE:
• Conditioning: 3 mL EtAc,
3 mL n-hexane,
6 mL MeOH,
9 mL H
2 O
• Sample
• Washing: 6 mL water
• Drying
Elution: 3 mL MeOH
• 1 mL of 98% H
2 SO
4 , 1 h,
75
C
• External quality
control: yes
• Population: occupational exposure
(n
¼ 8), Germany
[6]
ClF3CA (LLOQ
0.06); DF, nd
cis-DCCA
(LLOQ
0.08); DF, nd
trans-DCCA
(LLOQ
0.08); DF, nd
DBCA (LLOQ 0.06);
DF, nd
3PBA (LLOQ 0.06);
DF, nd
V: 0.4 mL
H: Enzymatic
E: MEPS (C18, SGE)
I: LVI-GC-MS (ion trap,
μSIS)
SPE (MEPS):
• Conditioning: 4
 50
μL
MeOH, 3
 20
μL 2% HCOOH
• Sample: 5
 100
μL
• Washing: 3
 50
μL 30%
MeOH
• Drying under vacuum
• Elution: 2
 40
μL 1%HFIP
and 2%DIIC in hexane
• 1% HFIP, 2% DIIC in hexane
• External quality
control: G-EQUAS
[17]
64
B. Wielgomas et al.