USA Clinical Laboratory needed that can perform GC analysis of human urine samples using the following procedure:
Startign Urine Sample
Incubate with urease - 30 minutes
Add ethanol or methanol, mix, centrifuge, and collect supernatant, dry under nitrogen or freeze-dry
Add methoxamine hydrochloride and incubate for up to 2 hours
Derivatize using MSFTA with 1% TMCS (30 to 60 minutes)
Analyze using GC
Use helium as the carrier gas at 1.5 ml min- 1 and set the injector split ratio to 1:20.
Maintain the injector, transfer line and ion source temperature at 220 °C, 200 °C and 250 °C, respectively, throughout each analysis.
Program oven temperature at 70 °C for 0.2 min, increase at 10 °C min- 1 to 270 °C and hold at 270 °C for 10 min.
OPTIONAL - If a TOF/MS detector is available, operate the MS EI mode (70 eV). Perform data acquisition in the full scan mode from m/z 40 to 600 with a solvent cutoff of 360 s and acquisition rate of 20 Hz. Set manual mass defect to 0 and detector voltage to between 1,700 and 1,800 V, depending on the detector's age and condition.
Perform sample injections using an autosampler if available
Perform three and five cycles of syringe washes before and after sample injection, respectively, using toluene as the wash solvent.
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