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.
DBCA (0.833; 2.5);
DF, nd
3PBA (0.008; 0.025);
DF, 30–35%
4F3PBA (0.017;
0.05); DF, 20–25%
V: 10 mL
H: acidic
E: LLE
I: GC-MS/MS (triple
quadrupole)
LLE
• Extraction: 20 mL
isopropanol-hexane (5:95)
• Evaporation to dryness
• 0.5 mL toluene + 20
μL
MTBSTFA (75
C, 45 min)
• Population:
20 adults and 20 children without occupational exposure
(China)
[26]
cis-DCCA
(0.1; nd);
DF, 95.3%
trans-DCCA
(0.1;
nd); DF, 98.3%
3PBA (0.1; nd); DF,
98.8%
V: 5 mL
H: acidic (1 mL HCl; 1 h,
90
C)
E: LLE
C: LLE
I: GC-MS (quadrupole,
SIM)
LLE:
• Extraction: 2
 4 mL hexane
• Evaporation (gentle stream of
nitrogen)
• Derivatization: 3 mL 10%
H
2 SO
4 in MeOH (75
C, 1 h)
Cleanup LLE:
• Re-extraction: 3 mL hexane
+3 mL saturated NaCl solution
• Evaporation (gentle stream of
nitrogen)
• Reconstitution: 100
μL of
toluene
• 3 mL 10% H
2 SO
4 in MeOH
(75
C, 1 h)
• Modification of
Kühn et al. [3]
• Population: pregnant women in an
agricultural area of
the Province of
Jiangsu (n
¼ 1,149),
China
[23]
cis-DCCA
(nd; 0.01);
DF, 100%
trans-DCCA
(nd;
0.01); DF, 100%
cis-DBCA
(nd; 0.01);
DF, 80%
4F3PBA (nd; 0.01);
DF, 5%
V: 5 mL
H: acidic (1 mL HCl; 1 h,
90
C)
E: LLE
C: LLE
I: GC-MS/MS (quadrupole, EI)
LLE:
• Extraction: 2
 5 mL hexane
• Cleanup: 2 mL 0.1 N NaOH
• Re-extraction: +0.1 mL conc.
HCl + 1.8 mL hexane
• Evaporation under nitrogen to
50
μL
MTBSTFA (10
μL)
• 80
C, 1 h
• External quality
control: G-EQUAS
• Population: general with no known
exposure to synthetic
pyrethroids (n
¼ 38),
Germany
[9]
62
B. Wielgomas et al.