GC-MS

Method /conditions

Columns
Manufacturer specifications

Model no: agilent 19091J-433 325 0C Max

HP-5% phenyl Methyl siloxane

Capillary30.0m X250 micro m X 0.25micro m nominal

He flow

Set point actual

Pressure 7.65 psi

Flow 1.0 ml/min

Average velocity 36 cm /sec

OVEN
On set point 0C 50

Actual 0C 50
0
Oven ramp C/min Next0C Hold min Run time
Initial 50 2.00 2.00
Ramp-1 10.0 280oC 10.00 35.00
Ramp-2 0.00
Ramp-3
Ramp-4
Ramp-5
Post run 0 0.00 35.00

Oven configuration

Maximum 0C 300

Equilibration min .10

Inlets

Mode split

Split Split

Ratio 10:1 flow 10.0ml/min

Gas saver 20 ml/ min @2.00min

Methamphetamine and caffeine separation

Methamphetamine hydrochloride can be isolated from several adulterants and diluents by the use
of solvent washes. For example, ephedrine hydrochloride and pseudoephedrine hydrochloride can
be separated from methamphetamine based on differences in chloroform solubilities.
Methamphetamine is very soluble in chloroform while ephedrine and pseudoephedrine are not very
soluble in chloroform. These components can be separated from a mixture by collecting the
methamphetamine in the first couple of drops of a chloroform rinse. Another useful technique is
multiple solvent recrystallization. For example, nicotinamide, caffeine, and dimethylsulfone are
slightly soluble in ether whereas methamphetamine hydrochloride is practically insoluble. The
separation is accomplished by dissolving a mixture of methamphetamine and these diluents in 2 mL
of methanol followed by dilution with 40 mL ether. The methamphetamine hydrochloride will
precipitate out of the ether whereas the adulterants remain dissolved.