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Confirmatory Determination of Buprenorphine and Norbuprenorphine in Urine Using A High-Throughput LC-HRAM-MS/MS Forensic Methodology
M S t
t
ass pec rome ry
Resul
MS/MS l i
f
d i
Th S i
tifi ™ Q E ti ™
HPLC
ana ys s was per orme us ng a ermo c en c xac ve
R i
t
i
d
Plus Hybrid Quadrupole-Orbitrap MS operating in a targeted-MS2 (t-MS2)
unn ng
equ ppe
heated electrospray ionization (HESI) mode at a resolution of 17 500 and
sample c
nsitivity,
,
iti
i
i ti
d T bl 1 h th
t
i l i
li t
ng/mL for
pos ve on za on mo e. a e s ows e exac mass nc us on s
(1/
i
settings for BUP, NBUP, and their respective IS used to collect t-MS2
x we g
y injection
data Tables 2 & 3 highlight the MS/MS HESI source and method
Figure 3
t
d
.
t
ti l
d
analytes
aggere
parame ers, respec ve y, use .
(5 ng/mL)
the QCs
cycle time
/mL.
Table 1. Q Exactive Plus t-MS2 exact mass inclusion list of settings.
Matrix Ef
The abso
BUP) and
from six d
Anal te
Mass [m/ ]
Form la
Species
water sa
rine for law
y
z
u
from 30 0
opular
.
l i
the use of a
BUP
468 31084 C29H41NO4
H
re at ve r
.
+
samples r
e mass
1 – system
NBUP
414.26389 C25H35NO4
+H
H d l
e
y ro ys
BUP-d4
472.33594 C29H37NO4
+H
As a resu
113% of
NBUP-d3
417.28272 C25H32D3NO4
+H
t l f
con ro a
molecular
KS)
Table 2 Q Exactive Plus HESI II source parameters used
Figure 3
,
was
.
.
.
NBUP an
nor urines
prepared
d t
t d
HESI II Source Parameters
C:\Xcalibur\...\CH1a\SurCal-2-01
eu era e
5.0 cal
RT:
0.00 -0.30
SM:
7G
RT:0.05
AA:57527
NBUP-
Sheath Gas*
60
80
100
dance
SN:177
TX A beta-
40
60
ativeAbun
.
h C
Aux Gas*
15
0
20
Rel
RT:0.05
AA:27610
c orp.,
80
100
ndance
SN:129
sample
Sweep Gas*
0
20
40
60
ativeAbu
urine
TM
to
S
3
0
Rel
RT:0.05
AA:5049640
SN 8743
sample
pray Voltage
.5 kV
60
80
100
undance
:
Capillary Temp
350
0
C
20
40
elativeAb
d in 1M
.
0
R
RT:0.05
AA:2509319
SN:4462
This was
Aux Gas Heater Temp
450
0
C
60
80
100
bundance
pped with
.
20
40
RelativeA
S-Lens RF Level
70.0
0.00
0.05
0
for 10
*A bit
U it
0k rpm for
T bl 5
r rary n s
MS/MS
a e .
-
(%Diff,
and Cha
Table 3 Q Exactive Plus Targeted MS2 method properties used
.
-
.
Analy
idr
em.
Targeted-MS2 Properties
BU
Polarity
Positive