001_TOC.qxp - page 132

673
GCCHROMATOGRAMS |
CLINICAL, FORENSIC&TOXICOLOGY
Cocaine, Opiates
Cocaine&Metabolites (TMSDerivatives)
Rtx®-5
min. 2
4
6
8
10
12
14
16
GC_PH00254
5
3
4
Column:
Rtx
®
-5, 30m, 0.25mm ID, 0.25µm (cat.# 10223)
Sample:
1.0µL split injection of cocaine and cocainemetabolites
Oven temp.:
150°C to 320°C@ 10°C/min.
Inj./det. temp.:
250°C/300°C
Carrier gas:
helium
Linear velocity:
30cm/sec. set@ 50°C
FID sensitivity:
2.56 x 10
-10
AFS
Split ratio:
30:1
1. ecgoninemethyl ester (TMSI)
2. ecgonine (TMSI)
3. cocaine
4. coca ethylene
5. benzoylecgonine (TMSI)
2
1
Opiates (TMSDerivatives)
Rtx®-5
1 2
3
4
5
6
7,8
9 10
11
min.
4
5
6
7
8
9
10
11
12
GC_PH00233
1. meperidine
2. alphaprodine
3. methadone
4. levorphanol (TMS)
5. codeine (TMS)
6. hydrocodone
7. morphine (TMS)
8. hydromorphone (TMS)
9. oxycodone (TMS)
10. oxymorphone (TMS)
11. nalorphine (TMS)
Column:
Rtx
®
-5, 30m, 0.25mm ID, 0.25µm (cat.# 10223)
Sample:
2.0µL split injection of opiates
Conc:
2,000ng/µL
Oven temp.:
200°C to 325°C@ 7°C/min.
Inj./det. temp.:
250°C/300°C
Det. type:
MS
Ionization:
EI
Carrier gas:
helium
Mode:
full scan
Linear velocity:
30cm/sec. set@ 200°C
Split ratio:
50:1
CocaineandMetabolites (TMSDerivatives)
Rxi®-5SilMS (100ng/mL)
Column
Rxi
®
-5Sil MS, 30m, 0.25mm ID, 0.25µm (cat.# 13623)
Sample
Diluent:
Butyl chloride
Conc.:
100 ng/mL
Injection
Inj. Vol.:
1µL splitless (hold 1min.)
Liner:
SingleGooseneckw/Wool (cat.# 22286-200.1)
Inj.Temp.:
250 °C
Purge Flow:
20mL/min.
Oven
OvenTemp:
100 °C to 200 °C at 30 °C/min. to 300 °C at 15 °C/min.
Carrier Gas
He, constant linear velocity
Linear Velocity: 40 cm/sec., 12.5 psi, 86.2kPa@ 100 °C
Detector
MS
Mode:
SIM
Transfer Line
Temp.:
310 °C
SourceTemp.:
250 °C
Solvent Delay
Time:
4min.
TuneType:
PFTBA
IonizationMode: EI
Instrument
Shimadzu 2010GC&QP2010+MS
Notes
Sampleswere prepared as follows:
Standards brought to dryness under nitrogen, then 50µL
BSTFA+ 1%TMCS (cat.# 35606) added. 50µL pyridine
was then added, and sampleswere incubated at 70°C for
30min. After incubation, sampleswere dilutedwith butyl
chloride.
*Used as derivitazation check
GC_CF1149
NEW!
Peaks
m/z 1 m/z 2
m/z 3
1. Ecgoninemethyl ester
82
96
256
2. Ecgonine
82
96
356
3. Cocaine
82
182
303
4. Cocaethylene
82
196
317
5. Benzoylecgonine
82
96
346
6. Cannabinol*
409
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Mar 2011
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