nida 5 panel exactive...6 forensic toxicology use only sample preparation procedure: modified add is...
TRANSCRIPT
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Forensic Toxicology Use Only
Analysis of Expanded NIDA 5 panel
Using Exactive System
Kevin HeThermo Fisher Scientific
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2Forensic Toxicology Use Only
New Guidelines from SAMHSA for Confirmation
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3Forensic Toxicology Use Only
New cutoffs, added analytes
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4Forensic Toxicology Use Only
List of compounds, their m/zs and cutoff vales
Number Name Formula [M+H]+
IS M+H Cutoff (ng/mL) QC1 (-60%) QC2 (+25%)
1 Amphetamine C9H13N 137.11936 141.14298 250 100 312.5
2 Methamphetamine C10H15N 151.13496 155.15858 250 100 312.5
3 MDA C10H13NO2 181.10916 185.13278 250 100 312.5
4 MDMA C11H15NO2 195.12486 199.14848 250 100 312.5
5 MDEA C12H17NO2 209.14046 214.17026 250 100 312.5
6 Benzoylecgonine (BE) C16H19NO4 291.14596 293.15722 100 40 125
7 THCA (cTHC) C21H28O4 346.21336 348.22462 15 6 18.75
8 Phencyclidine (PCP) C17H25N 245.21326 249.23688 25 10 31.25
9 Morphine C17H19NO3 287.15106 289.16232 2000 800 2500
10 Codeine C18H21NO3 301.16666 303.17792 2000 800 250011 6-Acetylmorphine (6-MAM) C19H21NO4 329.16166 331.17292 10 4 12.5
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5Forensic Toxicology Use Only
Calibrators and Controls
Drug 1 2 3 4 5 6 7 8 9 IS
Amphetamine 2 5 10 20 50 100 200 1000 200
Methamphetamine 2 5 10 20 50 100 200 1000 200
MDA 2 5 10 20 50 100 200 1000 200
MDMA 2 5 10 20 50 100 200 1000 200
MDEA 2 5 10 20 50 100 200 1000 200
BE 2 5 10 20 50 100 200 1000 200
THCA 2 5 10 20 50 100 200 200
PCP 2 5 10 20 50 100 200 1000 200
Morphine 2 5 10 20 50 100 200 1000 4000 200
Codeine 2 5 10 20 50 100 200 1000 4000 200
6MAM 2 5 10 20 50 100 200 1000 200
Concentration of calibrators (ng/mL)
Drug Cutoff(ng/mL) QC1 (40%)(ng/mL) QC2 (125%)(ng/mL) IS (ng/mL)
Amphetamine 250 100 312.5 200
Methamphetamine 250 100 312.5 200
MDA 250 100 312.5 200
MDMA 250 100 312.5 200
MDEA 250 100 312.5 200
BE 100 40 125 200
THCA 15 6 18.75 200
PCP 25 10 31.25 200
Morphine 2000 800 2500 200
Codeine 2000 800 2500 200
6MAM 10 4 12.5 200
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6Forensic Toxicology Use Only
Sample Preparation Procedure: Modified
Add IS (4 µg/mL, 10 µL)
Add 180 µL MeOHAdd 180 µL MeOH
Transfer ~ 400 µL to glass insert,
10, 25 or 50 µL injection
Transfer ~ 400 µL to glass insert,
10, 25 or 50 µL injection
Urine 200 µL in LR plastic tube
Add Spike (10 µL, S1-9, QC1, Cutoff, QC2)
Mix, add glucuronidase (0.1 mL), 60 °C, 30min or longer
Vortex, stand for 20 min,
centrifuge for 5 min at 15K RCF
Note: 50 mL injection (10 mL raw urine equivalent)
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7Forensic Toxicology Use Only
LC Conditions
Hypersil Gold PFP 150 × 2.1 mm, 5 µm
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8Forensic Toxicology Use Only
Lockmass Setup
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9Forensic Toxicology Use Only
Amphetamine: Calibration Curve
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10Forensic Toxicology Use Only
Amphetamine: QC
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11Forensic Toxicology Use Only
Methamphetamine: Calibration Curve
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12Forensic Toxicology Use Only
Methamphetamine: QC
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MDA: Calibration Curve
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14Forensic Toxicology Use Only
MDA: QC
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15Forensic Toxicology Use Only
MDMA: Calibration Curve
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16Forensic Toxicology Use Only
MDMA: QC
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MDEA: Calibration Curve
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18Forensic Toxicology Use Only
MDEA: QC
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19Forensic Toxicology Use Only
BE: Calibration Curve
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20Forensic Toxicology Use Only
BE: QC
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21Forensic Toxicology Use Only
THCA: Calibration Curve
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22Forensic Toxicology Use Only
THCA: QC
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23Forensic Toxicology Use Only
PCP: Calibration Curve
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24Forensic Toxicology Use Only
PCP: QC
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25Forensic Toxicology Use Only
Morphine: Calibration Curve
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26Forensic Toxicology Use Only
Morphine: QC
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Codeine: Calibration Curve
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28Forensic Toxicology Use Only
Codeine: QC
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29Forensic Toxicology Use Only
6-MAM: Calibration Curve
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30Forensic Toxicology Use Only
6-MAM: QC
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31Forensic Toxicology Use Only
Conclusion
• One sample preparation and one injection for confirmatory testing of all
NIDA-5 drugs
• Excellent quantitation using 0.5 mL processed sample.