Table 3
(continued)
Analytes (LOD
ng/mL; LOQ
ng/mL); DF
Sample volume (V), hydrolysis
(H), extraction (E), cleanup (C),
instrument (I)
Extraction and cleanup details
Notice
Ref.
DF, nd
3PBA (0.1; nd);
DF, nd
TIS
– turbo ion spray atmospheric
pressure ionization
• Elution: 1.5 mL MeOH + 2 mL ACN
• Evaporation to dryness
• Reconstitution in 50
μL ACN
(reconstitution)
cis-DCCA
(14 fmol injected;
nd); DF, nd
trans-DCCA
(18 fmol injected;
nd); DF, nd
3PBA (31 fmol
injected; nd); DF,
nd
LODs range: 0.1–
0.3 ng/mL
V: 5 mL
H: enzymatic
E: SPE (Sep-Pak C18 cartridges;
waters)
C: No
I: UHPLC- MS Q-TOF (ESI-)
SPE:
• Conditioning: 4 mL MeOH, 8 mL
water
• Sample
• Washing: 8 mL water
• Elution: 8 mL MeOH
• Evaporation
– gentle stream of
nitrogen
• Reconstitution in 1 mL MeOH
None
[32, 35,
36]
MPA (2.5 ng/mL);
DF, nd
3PBA (2.5 ng/
mL); DF, nd
V: 10 mL
H: acidic (HCl, conditions not
specified)
E: LLE
C: LLE
I: HPLC-UV
LLE:
• 10 mL of urine, 0.1 mL HCl, 2 mL
chloroform
• Organic phase, 0.1 mL 4 M NaOH,
1 mL water
• 0.5 mL aqueous phase, 0.5 mL HPLC
mobile phase (ACN:1% H
2 SO
4 ; 1:1)
• Large sample volume
• Not applicable for the measurement of
environmental exposure levels
[27]
3PBA (0.02; nd);
DF, 97.8%
V: 1 mL
H: acidic (6 M HCl; 2 h, 100
C)
E: SPE (OASIS HLB 150 mg/
6 cc, waters)
C: No
I: HPLC-MS/MS
SPE:
• Conditioning: MeOH, water
• Sample
• Washing: 5% MeOH
• Drying
• Elution: MeOH
• Evaporation
• Reconstitution in 100
μL ACN
• Based on Baker et al. [29]
• Population: pregnant women in the
first
trimester of gestation (n
¼ 231), Japan
[31]
70
B. Wielgomas et al.