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Cocaine and Metabolites (TMS Derivatives) on Rxi-5Sil MS (100 ng/mL)

GC_CF1149
Peaks m/z 1m/z 2m/z 3
1.Ecgonine methyl ester8296256
2.Ecgonine8296356
3.Cocaine82182303
4.Cocaethylene82196317
5.Benzoylecgonine8296346
6.Cannabinol*409----
*Cannabinol was used as a derivatization check.
ColumnRxi-5Sil MS, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13623)
Standard/Sample
Diluent:Butyl chloride
Conc.:100 ng/mL
Injection
Inj. Vol.:1 µL splitless (hold 1 min)
Liner:Single taper w/wool (cat.# 22286-200.1)
Inj. Temp.:250 °C
Purge Flow:20 mL/min
Oven
Oven Temp.:100 °C to 200 °C at 30 °C/min to 300 °C at 15 °C/min
Carrier GasHe, constant linear velocity
Linear Velocity:40 cm/sec, 12.5 psi, 86.2 kPa @ 100 °C
DetectorMS
Mode:SIM
Transfer Line Temp.:310 °C
Source Temp.:250 °C
Solvent Delay Time:4 min
Tune Type:PFTBA
Ionization Mode:EI
InstrumentShimadzu 2010 GC & QP2010+ MS
Sample PreparationStandards brought to dryness under nitrogen, then 50 µL BSTFA + 1% TMCS (cat.# 35606) were added. 50 µL pyridine was then added, and samples were incubated at 70 °C for 30 min. After incubation, samples were diluted with butyl chloride.
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