Table 2
(continued)
Pharmaceuticals
ASE extraction conditions
Clean-up
Analysis
References
Soil
mass
(g)
Solvent
T (
C)
P(psi or
bar)
Static extraction
time
(min)
 number
of cycles
Flush
volume
(%)
Cell matrix
(dispersant)
Recovery
(%)
RSD
(%)
LOD
Instrument
oxytetracycline, doxycycline, erythromycin,
roxithromycin
pH adjusted to
4.7 by NaOH
Chlortetracycline and oxytetracycline, and their TPs:
4-epitetracycline,
4-epianhydrotetracycline,
4-epichlorotetracycline,
epioxytetracycline,
α-apo-oxytetracycline, and
β-apo-oxytetracycline
5 g
Methanol/water
(3:1, v/v)
containing
25 mM EDTA
and 0.6 M
sodium chloride
(pH 8.0)
Room
T
C
10 MPa
20 min
 2
60%
HydromatrixVR
diatomaceous
earth
Tandem
SAX-HLB
SPE
cartridges
41%–110%
0.12–
0.34%
0.08–0.3 mg/g
HPLC-MS
[59]
Methylparaben, methyl
protocatechuate,
propylparaben,
3,4-dihydroxybenzoic acid,
4-hydroxybenzoic acid,
1,3,7-trimethylxanthine
(caffeine),
1,7-dimethylxanthine, carbamazepine,
3-hydroxycarbamazepine,
10,11-dihydro-10hydroxycarbamazepine, carbamazepine-10,11-epoxide,
diclofenac,
4-hydroxydiclofenac, ibuprofen, 1-hydroxyibuprofen,
2-hydroxyibuprofen,
carboxyibuprofen, sulfamethoxazole, and
N4-acetylsulfamethoxazole
2 g
MeOH (0.5%
v/v, formic acid)
50
C
1,500 psi
5 min
 2
60%
Diatomaceous
earth
In-cell
clean-up
with C18
and PSA
60–103%
<11%
0.04–4.31 ng/g
HPLC-MS/
MS
[69]
Sulfisomidine,
sulfamerazine,
sulfacetamide, sulfadoxine,
sulfabenzamide,
5 g
MeOH-water
(90:10, v/v)
100
C
1,500 psi
5 min
 3
100%
Hydromatrix
HLB
cartridges
60–130%
< 23%
0.01–4.19 ng/g
HPLC-MS/
MS
[61]
428
R. Manasfi et al.