Biomedical Engineering Reference
In-Depth Information
Table 1
(continu
ed)
IM/analyzer
(detection
mode)
Author, year [Ref]
Compounds
IS
Sample
Extraction procedure
Stationary phase
Mobile phase
Method validation
Gutteck et al.,
2003 [
108
]
Amitriptyline, citalopram,
clomipramine, desipramine,
dibenzepin, doxepin,
escitalopram, fl uvoxamine,
imipramine, opipramol,
reboxetine, trimipramine
(and some metabo-
lites) + fi ve neuroleptic
drugs
Imipramine-d3,
clomipramine-
d3, doxepin-d3,
chlorohaloperidol
Serum (1 mL)
LLE:
n
-hexane/DCM
(4:1) or DCM,
and different
reconstitution
volumen
depending on
analytes group
Silice Uptisphere C18
(125 × 2 mm, 5 m m)
Guard column
(8 × 2 mm)
50 mM
ammonium
formate pH 4/
ACN
ESI+/Q (SIM)
-
Selectivity
-
LLOQ = 1.2-54 nmol/L
-
Linearity: 2.3/540 to
46/5,400 nmol/L;
r
2
> 0.99
Intra-/inter-day
imprecision: %CV < 15%
-
Intra-/inter-day
inaccuracy: MRE ± 15%
-
Proccess ef fi ciency:
60-103%
-
Application to real
specimens
Halvorsen et al.,
2003 [
65
]
Amitriptyline,
clomipramine,doxepin,
trimipramine, citalopram,
fl uoxetine, fl uvoxamine,
paroxetine
Paroxetine
Plasma and
whole
blood
(0.05 mL)
LPME: 0.2M formic
acid(aceptor)/
dodecyl acetate
(organic solvent)
Inertsil 3 ODS-3 RP
(50 × 3mm, 3 m m)
5 mM
ammonium
formate
pH 2.7/ACN
ESI+/IT
(full scan,
m/z
260-335)
-
LLOQ = 1-106 ng/mL
-
Intra-/inter-day
imprecision:
%CV = 11-36%
-
Intra-/inter-day
inaccuracy: MRE ± 15%
-
Relative recovery: 9-75%
-
Matrix effect (post-col-
umn infusion experiment)
Juan et al.,
2005 [
66
]
Fluoxetine, citalopram,
venlafaxine, paroxetine
Fluvoxamine
Plasma
(0.5 mL)
SPE: Oasis HLB
(Auto Science
AP-0IP vacuum
pump)
Macherey-Nagel C18
(250 × 4.6 mm, 5 m m)
30 mM
ammonium
acetate (0.06%
formic acid)/
ACN
ESI+/Q
(SIM)
- Selectivity
- LOD = 0.1-0.5 ng/mL
- Linearity: 5-1000 ng/mL;
r
2
> 0.99
- Intra-/inter-day
imprecision: %CV < 15%
-
Intra-/inter-day
inaccuracy: MRE ± 15%
-
Absolute recovery >73%
-
Carry over
-
Stability (20°C/24h and
-20°C/3 months)
-
Application to real
specimens
