Eqiupment: GC instrument (Shimadzu GC-2010)
Column: DB-17 Agilent 30mX0.53mmX1.0μm
Initial oven temperature: 80℃
Initial time 2.0min
Rate 15℃/min
Final oven temperature: 250℃
Final time 20min
Carrier gas Nitrogen
Mode Constant flow
Flow 5.0mL/min
Split ratio 10:1
Injector temperature: 250℃
Detector temperature: 300℃
Injection volume 1.0μL
Precautions to be taken before analysis:
1. Condition column at 240℃ for minimum 30minutes.
2. Wash the syringe and clean injector liner properly to remove the contaminants of earlier analysis.
3. Wash, dry and fill diluent in syringe wash vials.
Diluent preparation:
Prepare 2% w/v sodium hydroxide solution in water.
Standard preparation:
Weigh about 100mg of (R)-3-hydroxyprrolidine hydrochloride standard into a vial, add 1mL of diluent and dissolve.
Test preparation:
Weigh about 100mg of test sample into a vial, add 1mL of diluent and dissolve. Prepare in duplicate.
Procedure:
Inject blank (diluent), standard preparation and test preparation using above GC conditions. Disregard the peaks due to blank. The retention time of peak due to (R)-3-hydroxyprrolidine is about 5.0min.
Note:
Report the result as an average
Post time: Nov-13-2021