General Test Procedure for Determination of Ethylene Glycol & Diethylene Glycol in Pharmaceutical Oral Dosage

1. Ethylene Glycol
IUPAC Name: Ethane-1,2-diol
CAS Number: 107-21-1
Molecular Weight: 64.053 g/mol
Molecular Formula: C2H6O2

2. Diethylene Glycol
IUPAC Name: 2-(2-hydroxyethoxy) ethanol
CAS Number: 111-46-6
Molecular Weight: 106.12
Molecular Formula: C4H10O3

Determination of Diethylene Glycol & Ethylene Glycol
Diluent: Acetone (GC Grade)
Impurity stock solution (Ethylene glycol): Weight accurately 100.0mg of ethylene glycol impurity transfer in to a 100 ml volumetric flask and volume with acetone and filter.
Impurity stock solution (Diethylene glycol): Weight accurately 100.0mg of diethylene glycol impurity transfer in to a 100 ml volumetric flask and volume with acetone and filter.
Impurity Standard Solution: 5 ml of each resulting solution dilute to 100 ml volume with acetone.
Test Solution: Weight accurately transfer about 5.88g or 5ml of sample in to 100 ml volumetric flask volume with acetone and mix properly. And filter.

Chromatography System
Mode: Gas chromatography
Detector: Flame Ionization
Column: 0.53 mm x 30 m Fused-silica analytical column coated with 1.8µm; DB-624 or any equivalent.
Injector Temperature: 220°C
Detector Temperature: 250°C

Initial Temperature

Temperature Ramp (áµ’/min)

Final Temperature (áµ’C)

Hold Time at Final Temperature (min)

60

-

60

4

60

50

120

10

120

50

220

6










Column: See the temperature program table
Carrier gas: Nitrogen
Injection size: 1.0µl
Flow Rate: 4.5 ml/min
Spilt Ratio: 10:1
Batch Table

Sr. No

Name of Injection

Injection No

Injection Volume

1

Blank Solution

01

1 µl

2

Impurity Standard –Ethylene Glycol solution & Diethylene Glycol solution

05

1 µl

3

Test Solution

02

1 µl


System Suitability requirement
System Suitability solution: Impurity Standard Solution
Relative Standard Deviation: Not more than 10% Ethylene Glycol solution & Diethylene Glycol solution

Calculation

Limit: 
Not more than 0.1 % of Ethylene glycol & Not more than 0.1% of Diethylene glycol

Post a Comment

Previous Post Next Post
close