SOP for Bracketing standard during Analysis of sample by Gas and Liquid Chromatography
1.0 OBJECTIVE :
To provide the procedure for bracketing during Analysis of sample by using Gas and Liquid chromatography i.e. HPLC, GC etc. to demonstrate the system suitability through the run of analysis for which the bracketing procedure is not given in the Technical Analytical Document (TAD).
2.0 SCOPE :
The scope of the SOP covers the procedure for doing the Bracketing during Analysis of sample by using Gas and Liquid chromatography i.e. HPLC, GC etc. to demonstrate the system suitability through the run of analysis at Quality control laboratory.
3.0 RESPONSIBILITY :
3.1 Quality Control for implementation.
3.2 Quality Control Head to ensure compliance.
4.0 PROCEDURE :
4.1 After conforming the system is suitable by injecting blank and system suitability solutions (if any), perform the analysis using bracketing system as follows.
4.2 Unless and otherwise specified in individual method inject six standard injection and at every bracketing stage perform two bracketing standard with one system suitability injection (if specified in individual method).
4.3 Relative Standard deviation (RSD) in case of bracketing standard to be considered as per Annexure – I if not specified in individual method and follow the criteria specified in method for system suitability injection if any.
4.4 After every 20 samples perform two bracketing standard with one system suitability injection (if specified in individual method).
Note: In case of Dissolution the number of injection for bracketing are 18 instead of 20.
4.5 When number of injections are less or more than 20 samples (i.e. at the end of analysis) perform two bracketing standard with one system suitability injection (if specified in individual method) at the end of analysis.
4.6 RSD of bracketing standard to be calculate as follows.
4.6.1 Consider all injection of standard solution including bracketing standard for calculation of RSD.
4.7 In a long sequence if RSD of bracketing standards and system suitability injection not meet the acceptance criteria for the samples consider the analysis up to previous bracketing of samples and repeat the analysis of those samples as fresh analysis.
4.8 For calculation purpose, average mean of initial six standards (or otherwise specified in method) is to be considered (if require)
4.9 Schematically it is reported as follows.
|
1.0 |
Blank |
|
2.0 |
System suitability (if any ) |
|
3.0 |
Standard Injection 1 |
|
4.0 |
Standard Injection 2 |
|
5.0 |
Standard Injection 3 |
|
6.0 |
Standard Injection 4 |
|
7.0 |
Standard Injection 5 |
|
8.0 |
Standard Injection 6 |
|
9.0 |
Test Injection 1 |
|
10.0 |
Test Injection 2 |
|
11.0 |
Test Injection 3 |
|
12.0 |
Test Injection 4 |
|
13.0 |
Test Injection 5 |
|
14.0 |
Test Injection 6 |
|
15.0 |
Test Injection 7 |
|
16.0 |
Test Injection 8 |
|
17.0 |
Test Injection 9 |
|
18.0 |
Test Injection 10 |
|
19.0 |
Test Injection 11 |
|
20.0 |
Test Injection 12 |
|
21.0 |
Test Injection 13 |
|
22.0 |
Test Injection 14 |
|
23.0 |
Test Injection 15 |
|
24.0 |
Test Injection 16 |
|
25.0 |
Test Injection 17 |
|
26.0 |
Test Injection 18 |
|
27.0 |
Test Injection 19 * |
|
28.0 |
Test Injection 20 * |
|
29.0 |
Standard Injection 1 |
|
30.0 |
Standard Injection 2 |
|
31.0 |
Resolution Solution if any specified in method |
|
|
2 Standard Injection and system suitability if specified in method (At the end of complete analysis) if it complete before the regular cycle of 20* sample analysis followed by bracketing. |
* – 18 injection in case of dissolution
5.0 ANNEXURE(S):
Annexure I: Limit Of Relative Standard Deviation (RSD) for Bracketing Standards
1. Assay, Content Uniformity, Dissolution By HPLC – RSD limit is NMT 2.0 % if the number of standards are less than or equal to 5. RSD limit is NMT 3.0 % if the number of standards are more than 5.
2. Related Substance or Related Compound or Degradant Products By HPLC – RSD limit is NMT 5.0 %
3. Analysis By GC – RSD limit is NMT 15.0 %