Chapter 6 Experimental Work
ACETATE BY HPLC
Method of Analysis
Mobile phase: 0.025 mol/L (0.05N) sulfuric Acid. Using a volumetric pipette, add 3 ml of concentrated sulfuric acid to approx. 1500 ml water in 2 liter volumetric flask. Dilute volume with water.
Standard Preparations: Accurately weigh 0.240g each std1 and std2 of sodium acetate tri-hydrate W.S. into 100 ml volumetric flask. Then dilute 25 ml to 50 ml with water.
Sample Preparation: Dilute with water such that the concentrated of the sample lies within the concentrated range of the appropriate working standards for Plasma-Lyte A injection. Pipette 25 ml to a 100 ml volumetric flask and dilute to volume. HPLC Parameters:
Mobile phase: 0.05N Sulfuric acid
Injection …show more content…
Acceptance criteria
There should no interference from Blank solution and Placebo. The RT of the sample shall be corresponds with RT of standard in specificity preparation.
PRECISION
Procedure
Method of analysis follows as per specificity parameter except run time. Run time may be adjusted based on the above analysis.
To demonstrate the method of precision six samples were prepared as per the test method representing a single batch. Determine the assay of these samples and evaluate the precision of the method by the % RSD of the assay results.
Table 3 Precision – Sequence of Injection
S.No. Name of the Sample No. of Injections
1 Blank 1
2 Standard 1 6
3 Standard 2 2
4 Sample 1 2
5 Sample 2 2
6 Sample 3 2
7 Sample 4 2
8 Sample 5 2
9 Sample 6
ACETATE BY HPLC
Method of Analysis
Mobile phase: 0.025 mol/L (0.05N) sulfuric Acid. Using a volumetric pipette, add 3 ml of concentrated sulfuric acid to approx. 1500 ml water in 2 liter volumetric flask. Dilute volume with water.
Standard Preparations: Accurately weigh 0.240g each std1 and std2 of sodium acetate tri-hydrate W.S. into 100 ml volumetric flask. Then dilute 25 ml to 50 ml with water.
Sample Preparation: Dilute with water such that the concentrated of the sample lies within the concentrated range of the appropriate working standards for Plasma-Lyte A injection. Pipette 25 ml to a 100 ml volumetric flask and dilute to volume. HPLC Parameters:
Mobile phase: 0.05N Sulfuric acid
Injection …show more content…
Acceptance criteria
There should no interference from Blank solution and Placebo. The RT of the sample shall be corresponds with RT of standard in specificity preparation.
PRECISION
Procedure
Method of analysis follows as per specificity parameter except run time. Run time may be adjusted based on the above analysis.
To demonstrate the method of precision six samples were prepared as per the test method representing a single batch. Determine the assay of these samples and evaluate the precision of the method by the % RSD of the assay results.
Table 3 Precision – Sequence of Injection
S.No. Name of the Sample No. of Injections
1 Blank 1
2 Standard 1 6
3 Standard 2 2
4 Sample 1 2
5 Sample 2 2
6 Sample 3 2
7 Sample 4 2
8 Sample 5 2
9 Sample 6