restektn07 - page 224

CLINICAL/FORENSICS
13
Cocaine; Phencyclidine
GC
GC
HPLC
Cocaine
Benzoylecgonine is themajormetabolite found inurine after cocaine abuse.Monitoring for benzoylecgonine is required in the
testing protocol established by the Department of Health and Human Services and the National Institute on Drug Abuse.
Benzoylecgonine and other cocaine metabolites should be derivatized prior to analysis. Parent cocaine and its derivatized
metabolites canbeanalyzed togetheronanRtx®-5columnwithgoodpeak shapeand resolution.Theanalysisalsocanbeaccom-
plishedbyHPLC.
Phencyclidine
Phencyclidine can be screened for using immunoassay tech-
niques. However, prior to reporting positive results, the pres-
ence of phencyclidine should be confirmed by an alternative
chemical test.Phencyclidineeasilycanbechromatographedon
phenylmethyl stationary phases like Rtx®-5. Low picogram
amounts of the drug canbe detectedbyNPDorGC/MS.
Cocaine&Metabolites (TMSDerivatives)
Rtx®-5
min. 2
4
6
8
10
12
14
16
GC_PH00254
2
1
5
3
4
30m, 0.25mm ID, 0.25µmRtx
®
-5 (cat.# 10223)
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 (TMS)
2. ecgonine (TMS)
3. cocaine
4. coca ethylene
5. benzoylecgonine (TMS)
Phencyclidine (PCP)
Rtx®-5
30m, 0.25mm ID, 0.25µmRtx
®
-5 (cat.# 10223)
1.0µL split injection of phencyclidine
Conc.:
1000ng/µL
Oven temp.:
50°C (hold 1min.) to 250°C@ 25°C/min.,
then to 325°C@ 10°C/min. (hold 2min.)
Inj. / det. temp.:
250°C / 325°C
Carrier gas:
helium
Linear velocity:
30cm/sec. set@ 50°C
FID sensitivity:
2.56 x 10
-10
AFS
Split ratio:
30:1
min. 2
4
6
8
10
12
14
16
18
GC_PH00234
1. phencyclidine
1
CocaineandEcgonineMethylEster
Allure™PFPPropyl
Peak List:
1. EME (ecgoninemethyl ester)
2. COC (cocaine)
Sample:
Inj.:
10µL
Conc.:
1µg/mL
Solvent:
water
Temp.:
4°C
Column:
Allure™PFPPropyl
Cat.#:
9169532
Dimensions: 30 x 2.1mm
Particle size: 5µm
Pore size: 60Å
Data Courtesy of ShaneNeedham, Pfizer Inc.
LC_0126
XIC of+MRM (3 pairs) for
304.0 / 182.0 amu
2.35e3 cps
2
0
0.5 1.0 1.5 2.0 2.5 3.0
3.5 4.0 4.5
min.
XIC of+MRM (3 pairs) for
200.0 / 182.0 amu
1.30e3 cps
1
0
0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
min.
Conditions:
Mobile phase:
5mM ammonium
formate, pH 3.0:
acetonitrile (10:90, v/v)
Flow:
0.6mL/min.
Column temp.:
ambient
Det.:
PE/Sciex API 3000
Interface:
turbo ion spray, ESI
Interface temp.:
150°C
Ionmode:
positive
ESI probe voltage:
5000V
Orifice:
+ 71V
Ring:
+ 265V
Collision gas:
nitrogen
Collision gas pressure:
2.2mTorr
Collision gas energy:
28 eV (COC)
26 eV (EME)
Electronmultiplier:
2100 volts
Auxilary gas flow:
7000cc/min.
Nebulizer gas setting:
15lb/in.²
Curtain gas setting:
12lb/in.²
free
literature
HPLCColumn SelectionGuide
lit. cat.# 59454B
Allure
PFPPropyl andUltraPFPColumns Provide Improved
Analyses of Basic Compounds
lit. cat.# 59118A
Call Restek at 800-356-1688 or 814-353-1300, ext. 5, or contact
your Restek representative, to request your free copy!
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