Fentanyl, Metabolite, and Analogues in Urine on Rap€¦ · Fentanyl, Metabolite, and Analogues in...
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Restek Corporation 110 Benner Circle Bellefonte, PA 16823 1-814-353-1300 • 1-800-356-1688 • Fax: 1-814-353-1309 • www.restek.com LC_CF0591 Fentanyl, Metabolite, and Analogues in Urine on Raptor™ Biphenyl by LC-MS/MS Column Raptor ™ Biphenyl (cat.# 9309552) Dimensions: 50 mm x 2.1 mm ID Particle Size: 5 μm Temp.: 30 °C Sample Conc.: A 10 ng/mL standard was prepared in urine. The internal standard was fortified to a final concentration of 1 ng/mL. An 80 μL aliquot of the 10 ng/mL urine standard was diluted with 320 μL of 70:30 water:methanol solution (5-fold dilution) prior to analysis. Inj. Vol.: 5 μL Mobile Phase A: 0.1% Formic acid in water B: 0.1% Formic acid in methanol Time (min) Flow (mL/min) %A %B 0.00 0.4 70 30 2.00 0.4 20 80 2.01 0.4 70 30 3.50 0.4 70 30 Detector MS/MS Ion Mode: ESI+ Instrument HPLC Conc. Peaks tR (min) (ng/mL) Q1 Q3 Quantifier Q3 Qualifier 1. Norfentanyl 1.04 10 233.10 84.08 150.11 2. Norfentanyl-d5 (IS) 1.02 1 238.10 84.08 — 3. Acetyl fentanyl 1.48 10 323.29 188.18 105.10 4. Acetyl fentanyl-13C6 1.48 1 329.22 188.22 — 5. Fentanyl 1.65 10 337.29 188.22 105.09 6. Fentanyl-d5 (IS) 1.64 1 342.35 188.22 — 7. Sufentanil 1.84 10 387.35 238.18 111.07 8. Sufentanil-d5 (IS) 1.83 1 392.29 238.18 — 0.0 1,2 3,4 5,6 7,8 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 Time (min) !"! #! $% !"! #! !! &’()
Transcript of Fentanyl, Metabolite, and Analogues in Urine on Rap€¦ · Fentanyl, Metabolite, and Analogues in...
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est
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m
LC_
CF0
59
1
Fe
nta
ny
l, M
eta
bo
lite
, an
d A
na
log
ue
s in
Uri
ne
on
Ra
pto
r™ B
iph
en
yl
by
LC
-MS
/MS
Col
umn
Rapt
or ™
Bip
heny
l (ca
t.# 9
3095
52)
Dim
ensi
ons:
50
mm
x 2
.1 m
m ID
Part
icle
Siz
e:
5 µm
Tem
p.:
30 °C
Sam
ple
Conc
.: A
10
ng/m
L st
anda
rd w
as p
repa
red
in u
rine.
The
inte
rnal
sta
ndar
d w
as fo
rtifi
ed to
a fi
nal
co
ncen
trat
ion
of 1
ng/
mL.
An
80 µ
L al
iquo
t of t
he 1
0 ng
/mL
urin
e st
anda
rd w
as d
ilute
d w
ith
32
0 µL
of 7
0:30
wat
er:m
etha
nol s
olut
ion
(5-f
old
dilu
tion)
prio
r to
anal
ysis
.In
j. Vo
l.:
5 µL
Mob
ile P
hase
A
: 0.
1% F
orm
ic a
cid
in w
ater
B:
0.1%
For
mic
aci
d in
met
hano
l
Tim
e (m
in)
Flow
(mL/
min
) %
A
%B
0.
00
0.4
70
30
2.00
0.
4 20
80
2.
01
0.4
70
30
3.50
0.
4 70
30
Det
ecto
r M
S/M
SIo
n M
ode:
ES
I+In
stru
men
t H
PLC
Con
c.
Peak
s tR
(min
) (n
g/m
L)
Q1
Q3
Qua
ntifi
er
Q3
Qua
lifier
1.
N
orfe
ntan
yl
1.04
10
23
3.10
84
.08
150.
11
2.
Nor
fent
anyl
-d5
(IS)
1.02
1
238.
10
84.0
8 —
3.
A
cety
l fen
tany
l 1.
48
10
323.
29
188.
18
105.
10
4.
Ace
tyl f
enta
nyl-
13C6
1.
48
1 32
9.22
18
8.22
—
5.
Fe
ntan
yl
1.65
10
33
7.29
18
8.22
10
5.09
6.
Fe
ntan
yl-d
5 (IS
) 1.
64
1 34
2.35
18
8.22
—
7.
Su
fent
anil
1.84
10
38
7.35
23
8.18
11
1.07
8.
Su
fent
anil-
d5 (I
S)
1.83
1
392.
29
238.
18
—
0.0
1,2
3,4
5,6
7,8
0.20
0.40
0.60
0.80
1.00
1.20
1.40
1.60
1.80
2.00
Tim
e (m
in)
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