Biomedical Engineering Reference
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Table 3 Preparation of mammalian samples by liquid-liquid extraction (LLE) prior to LC-MS analysis
Sample:solvent
volume ratio b
Organic solvent a
Sample matrix
Analyte
Steps prior to LLE
Recovery (%)
Reference
C 5 H 12 /H 2 CCl 2 / iso prop
46:49:5
Rat urine, bile
Benz
n.s. (3×)
Lyophilization, +MeOH +PB, pH 7.2 c
n.s.
[ 59 ]
HCCl 3
Liver microsomes d
Cim
1:1.4 (2×)
+IS +NaCl +hepSA, pH 3.7
75
[ 23 ]
H 2 CCl 2
Hum plasma
S -Hyo
1:4.3
+IS +1 M NH 4 OH
110
[ 90 ]
H 2 CCl 2
Hum plasma
Cim
1:11.8
+IS
64
[ 61 ]
H 2 CCl 2
Hum plasma
BuS
1:8.6
+IS
69
[ 79 ]
H 2 CCl 2
Rat, mouse, hamster,
guinea pig liver
microsomes
Cim, metab.
1:1.4 (2×)
+IS +NaCl +hepSA, pH 3.7
62
[ 23 ]
H 2 CCl 2
Hum plasma
Tio
1:2
+IS +ACN (precipitation) e
76-81
[ 80 ]
H 2 CCl 2 / iso prop 4:1
Equine urine
Atr, Scp
1:0.73
+1 M NaOAc pH 5.0 +b-glucu +25 %
NH 4 OH f
n.s.
[ 14 ]
EE
Liver microsomes d
Cim
1:1.4 (2×)
+IS +NaCl +hepSA, pH 3.7
32
[ 23 ]
EE
Rat faeces
Ada, metab.
1:2
+0.001 % Na 2 CO 3
n.s.
[ 6 ]
EE
Rat liver homogenate
Ada, metab.
1:2
n.s.
[ 6 ]
EE
Rat faeces
Adi, metab.
1:2
+0.001 % Na 2 CO 3
n.s.
[ 5 ]
EE
Rat liver homogenate
Adi, metab.
1:2
n.s.
[ 5 ]
EE
Rat faeces
Atr, metab.
1:2
+0.001 % Na 2 CO 3
n.s.
[ 52 ]
EE
Rat faeces
Scp
1:2
+0.001 % Na 2 CO 3
n.s.
[ 87 ]
EE
Equine urine
Ipra
1:1
+IS +borax buffer +5 M NaOH, pH 10.0 g
82
[ 24 ]
EE
Hum plasma
Gran
1:6.3
+IS +0.1 M NaOH
98
[ 71 ]
EE/C 6 H 14 75:25
Dog, monkey urine
Beme (MDL
72,222), metab.
n.s. (2×)
Lyophilization, +acid, pH 2.0 or +base,
pH 10.0
n.s.
[ 37 ]
Et 2 O
Liver microsomes d
Cim
1:1.4 (2×)
+IS +NaCl +hepSA, pH 3.7
54
[ 23 ]
 
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