Biomedical Engineering Reference
In-Depth Information
Table 4
Preparation of mammalian samples by solid-phase extraction (SPE) prior to LC-MS analysis
SPE material
Sample matrix
Analyte
Previous step
Elution solvent
a
Recovery (%)
Reference
C18 (AccuBOND
II
)
Rat urine
Ada, metab.
None
MeOH
n.s.
[
6
]
C18 (AccuBOND
II
)
Rat urine
Adi, metab.
None
MeOH
n.s.
[
5
]
C18 (AccuBOND
II
)
Rat urine
Atr, metab.
Hydrolysis
b
, adjust pH 8.0
MeOH
n.s.
[
51,
52
]
C18 (AccuBOND
II
)
Rat urine
Scp, metab.
Hydrolysis
b
, adjust pH 8.0
MeOH
n.s.
[
7,
87
]
C18 (Sep-Pak)
Dog plasma
Atr
None
MeOH/0.1 M NH
4
OAc 3:1
107
[
96
]
C18 (Sep-Pak)
Rat, mouse, hamster,
guinea pig liver
microsomes
Cim, metab.
+1 % ZnSO
4
(precipitation)
MeOH
100
[
23,
62
]
C18 (Supelclean LC)
Hum plasma
Tio
+IS
MeOH/Et
3
N/HOAc 99:0.5:0.5
92
[
81
]
C8-SCX mixed mode
(Bond Elute certify)
Hum plasma
Atr, Scp
Adjust pH 3.0, +IS
MeOH/NH
4
OH 98:2
61-84
[
11
]
CBA Bond Elut LRC Hum blood
c
Ipra +PB, pH 8.0; +IS after SPE MeOH/1 M HCl 30:70 96-103 [
54
]
CBA ISOLUTE Equine urine Ipra, BuS +0.01 M (NH
4
)
2
CO
3
, pH 9.3 1 % FA in MeOH n.s. [
78
]
HLB Oasis Hum viscera Atr, Scp Leaching with PBS MeOH n.s. [
15
]
HLB Oasis Hum urine Atr +IS MeOH n.s. [
12
]
HLB Oasis Hum plasma Tros +IS +H
3
PO
4
2 mM NH
4
OAc/ACN 20:80 73 [
84
]
HLB Oasis
d
Hum serum Scp +IS +PB MeOH 51 [
97-
99
]
HLB Oasis
e
Rat plasma, brain Tros, Scp, MeS +PB, pH 8.0, +IS MeOH n.s. [
77
]
MCX Oasis Hum plasma
R/S
-Hyo +IS, +2 % FA 2.25 % NH
4
OH in MeOH 81-83 [
48
]
For abbreviation of analyte names see Sect. “Abbreviations”.
ACN
acetonitrile,
CBA
carboxylic acid,
FA
formic acid,
HLB
hydrophilic-lipophilic balance,
hum
human,
IS
internal standard,
LRC
large reservoir capacity,
MCX
mixed-mode cation exchange,
metab.
metabolites (biotransformation products produced
in vivo),
MeOH
methanol,
n.s.
not speci fi ed,
OAc
acetate,
PB
phosphate buffer,
PBS
phosphate-buffered saline,
SCX
strong cation exchange
a
Ratio given as v/v
b
Hydrolysis of phase II biotransformation products (conjugates) of TA was either done enzymatically (b-glucuronidase) or non-enzymatically under acidic
conditions
c
Human whole blood
d
Automated performance
e
In 96-well plate format
