Biomedical Engineering Reference
In-Depth Information
Author, year [Ref]
Compounds
IS
Sample
Extraction procedure
Stationary phase
Mobile phase
mode)
Method validation
Shinozuka et al.,
2006 [
69
]
Imipramine, desipramine,
amitriptyline, nortriptyline,
trimipramine, clomip-
ramine, lofepramine,
amoxapine, dosulepin,
maprotiline, mianserin,
setiptiline, trazodone,
fl uvoxamine, paroxetine,
milnacipram, sulpiride,
tandspirone, methylpheni-
date, melitracen
Diazepam
Plasma (1 mL)
SPE: Oasis HLB
Inertsil C8 (150 × 2 mm,
5 m m)
10 mM
ammonium
acetate pH5/
MeOH/ACN
SSI+/IT (full
scan,
m/z
60-500)
-
LOD = 30-630 ng/mL
-
LLOQ = 100-1,000 ng/mL
-
Linearity: 100-1,000 ng/
mL;
r
2
> 0.99
-
Intra-day imprecision:
%CV < 15%
-
Intra-day inaccuracy:
MRE ± 15%
-
Relative recovery >69%
Kirchherr et al.,
2006 [
53
]
Amitriptyline, imipramine,
trimipramine, clomip-
ramine, citalopram,
fl uoxetine, fl uvoxamine,
paroxetine, sertraline,
venlafaxine, reboxetine,
viloxazine, doxepin,
maprotiline, mianserine,
mirtazapine, moclobemide,
trazodone, opipramol
(and some metabolites)
+ antipsychotics
Clonidine,
dihydromethyl-
risperidone,
metabenztiaz-
urone
Serum
(0.1 mL)
Protein precipitation
(ACN/MeOH)
Collected
supernantat
volume and
dilution factor
depending on
therapeutic range
of analytes group
Chromolith Speed ROD
C18 monolithic
column (50 × 4.6 mm,
5 m m)
5 mM
ammonium
acetate
pH 3.9/MeOH
ESI+/QqQ
(MRM)
-
LLOQ = 0.03-28.3 ng/mL
-
Linearity: 1 to
20/50/100 ng/mL; 5/10 to
200/500/1,000 ng/mL,
100-10,000 ng/mL
(depending on therapeutic
range);
r
2
> 0.99
-
Intra-/inter-day
imprecision: %CV < 15%
-
Intra-/inter-day
inaccuracy: MRE ± 15%
-
Absolute recovery >90%
Sauvage et al.,
2006 [
76
]
Amitriptyline, imipramine,
desipramine, clomipramine,
trimipramine, amoxapine,
doxepin, maprotiline,
mianserin, dothiepin,
fl uoxetine, paroxetine,
sertraline, citalopram (and
some metabolites)
Mianserine-d3,
amitriptyline-d6,
clomipramine-d3,
imipramine-d3
Serum
(0.1 mL)
Protein precipitation
(ACN) Online
SPE: Cyclone
(50 × 0.5 mm,
50 m m)
XTerra MS C18
(50 × 2.1 mm, 5 m m)
0.1% formic
acid/ACN
(0.1% formic
acid)
ESI+/QqQ
(MRM)
-
Linearity: 10-500 ng/mL;
r
2
> 0.99
-
Intra-/inter-day
imprecision: %CV < 15%
-
Intra-/inter-day
inaccuracy: MRE ± 15%
-
Matrix effect (post-col-
umn infusion experiment)
-
Dilution integrity (1/2 and
1/10): %CV <15%
-
Carry over
-
External pro fi ciency test
-
Application to real
specimens
(continued)
