Table 2
ASE extraction and analysis conditions in soil
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
Diclofenac, allopurinol,
verapamil, carbamazepine,
spironolactone, salbutamol,
omeprazole, atenolol,
bendroflumethiazide, diltiazem, acetylsalicylic acid,
furosemide, prednisolone,
cyproterone acetate, erythromycin, enalapril, metoprolol, paracetamol, citalopram,
cimetidine, diazepam,
zopiclone, oxazepam,
amoxicillin, ramipril, terbutaline, penicillin G, ibuprofen, morphine, gestodene,
losartan potassium,
amlodipine besylate,
simvastatin
20 g
Methanol/aqueous ammonia
solution (0.1
mol L
À1
) (1:1, v:
v)
80
C
1,500 psi
5 min
 5
50%
Ottawa sand
Tandem
MAX-HLB
SPE
cartridges
66–114%
1–14%
0.1–<2.5 ng/g
LC-MS/MS
[64]
Chlortetracycline, oxytetracycline, sulfadiazine, erythromycin, and tylosin
(degradation products:
TYL A, B, C, and D)
10 g
Methanol/0.2 M
citric acid buffer
(pH 4.7 adjusted
with NaOH) (1:1,
v:v)
Room T
C
1,500 psi
10 min
 1
and 3 min
 1
100%
Ottawa sand
Tandem
SAX-HLB
SPE
cartridges
50–100%
Not
reported
0.6–5.6 g/kg
LC-MS/MS
[58]
Ciprofloxacin and
norfloxacin
0.5 g
50 mM aqueous
phosphoric acid
(pH 2.0) and acetonitrile mixture
(1:1, v/v)
100
C
100 bar
15 min
 6
150%
Quartz sand
MPC disk
cartridge
75–92%
8–11%
0.05 mg/kg of
dry matter
LC-FLD
[68]
Paracetamol, salicylic acid,
propranolol hydrochloride,
clofibric acid, ketoprofen,
diclofenac sodium salt,
bezafibrate, warfarin,
flurbiprofen, indomethacin,
ibuprofen sodium salt,
meclofenamic acid sodium
salt, gemfibrozil, atenolol,
salbutamol, sulfamethoxazole, sulfamethazine sodium
2.7 g
MeOH:H2O
(50:50, v/v)
60
C
1,500 psi
5 min
 2
100%
Sea sand
HLB
cartridges
>60% (for
20 analytes)
Not
reported
<20 ng/g (for
20 analytes)
LC-MS/MS
[55]
426
R. Manasfi et al.
ASE extraction and analysis conditions in soil
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
Diclofenac, allopurinol,
verapamil, carbamazepine,
spironolactone, salbutamol,
omeprazole, atenolol,
bendroflumethiazide, diltiazem, acetylsalicylic acid,
furosemide, prednisolone,
cyproterone acetate, erythromycin, enalapril, metoprolol, paracetamol, citalopram,
cimetidine, diazepam,
zopiclone, oxazepam,
amoxicillin, ramipril, terbutaline, penicillin G, ibuprofen, morphine, gestodene,
losartan potassium,
amlodipine besylate,
simvastatin
20 g
Methanol/aqueous ammonia
solution (0.1
mol L
À1
) (1:1, v:
v)
80
C
1,500 psi
5 min
 5
50%
Ottawa sand
Tandem
MAX-HLB
SPE
cartridges
66–114%
1–14%
0.1–<2.5 ng/g
LC-MS/MS
[64]
Chlortetracycline, oxytetracycline, sulfadiazine, erythromycin, and tylosin
(degradation products:
TYL A, B, C, and D)
10 g
Methanol/0.2 M
citric acid buffer
(pH 4.7 adjusted
with NaOH) (1:1,
v:v)
Room T
C
1,500 psi
10 min
 1
and 3 min
 1
100%
Ottawa sand
Tandem
SAX-HLB
SPE
cartridges
50–100%
Not
reported
0.6–5.6 g/kg
LC-MS/MS
[58]
Ciprofloxacin and
norfloxacin
0.5 g
50 mM aqueous
phosphoric acid
(pH 2.0) and acetonitrile mixture
(1:1, v/v)
100
C
100 bar
15 min
 6
150%
Quartz sand
MPC disk
cartridge
75–92%
8–11%
0.05 mg/kg of
dry matter
LC-FLD
[68]
Paracetamol, salicylic acid,
propranolol hydrochloride,
clofibric acid, ketoprofen,
diclofenac sodium salt,
bezafibrate, warfarin,
flurbiprofen, indomethacin,
ibuprofen sodium salt,
meclofenamic acid sodium
salt, gemfibrozil, atenolol,
salbutamol, sulfamethoxazole, sulfamethazine sodium
2.7 g
MeOH:H2O
(50:50, v/v)
60
C
1,500 psi
5 min
 2
100%
Sea sand
HLB
cartridges
>60% (for
20 analytes)
Not
reported
<20 ng/g (for
20 analytes)
LC-MS/MS
[55]
426
R. Manasfi et al.