Pyridine HCl Derivative Detection in Pantoprazole - Gas Chromatography
Project Description
ASIA / USA GMP contract pharmaceutical research lab needed for testing of “2-Chloro methyl-3,4-dimethoxy pyridine HCl content by GC” per the attached procedures on Pantoprazole.
3.2.S.4.2 ANALYTICAL PROCEDURES
2-Chloromethyl-3,4-dimethoxy pyridine hydrochloride in Pantoprazole sodium by GC:
Gas chromatography equipped with a μECD detector.
Column: 30 m × 0.53 mm fused silica column coated with 6%-Cyano propyl phenyl 94%-dimethyl poly siloxane, 3μm (Use DB-624 or equivalent).
Chromatographic conditions:
Injector temperature : 290°C
Detector temperature : 300°C
Detector flow (N2) : 60 ml/min
Column pressure : 10 psi
Carrier gas : Nitrogen
Injection mode : Split
Split ratio : 1:1
Injection volume : 4 μL
Oven program : Heat at 180°C for 1 minute and increase the temperature to 250°C at a rate of 10°C/min
Standard solution (5 ppm solution):
Weigh accurately about 12.5 mg of 2-chloromethyl-3, 4-dimethoxy pyridine hydrochloride working standard into a 25 ml volumetric flask, dissolve and take make up to volume with water. Take 10 μL of this solution in to a 100 ml volumetric flask, dilute to volume with n-Hexane.
Test solution:
Weigh accurately about 100 mg of sample and dissolve in 10 ml of 1N sodium hydroxide (heat if necessary). Transfer the solution into a separation funnel and add 10 ml of n-Hexane. Shake for 5 minutes. Allow the layers to separate and collect the upper organic phase. Transfer this solution into a GC vial.
Retention time of genotoxic impurity (2-chloromethyl-3, 4-dimethoxy pyridine hydrochloride) of Pantoprazole Sodium about 5.0 minutes.
Procedure:
After equilibration of the column inject single injection of blank, six replicate injections of standard solution, single injection of test solution single injection of bracketing standard in to the chromatograph.
Note: Repeat blank and bracketing standard for five test samples.
Project Information
Number:24-01896
Industry:Pharmaceuticals
