Procedure for Analytical method development of Residue method by using HPLC

1.0 OBJECTIVE

To lay down the Procedure for Residue Method Development.

2.0 SCOPE

This SOP is applicable to Develop the Residue method in Company.

3.0 BACKGROUND

NIL

4.0 RESPONSIBILITY

4.1 All Analytical Research to develop the Residue method.

4.2 Group leader Analytical Research to ensure the procedure is followed.

4.3 Head Analytical Research or his designee to ensure compliance.

5.0 PROCEDURE

5.1 Solubility profile:

Solubility information in different solvents shall be checked while selecting the diluents for Standard solutions and extraction solvents for test solutions.

5.2 Selection of a Detection method

In general, the detection method could be a HPLC method (Either Dissolution or Assay Method for that particular product).

5.3 Selection of Mobile phase composition:

Mobile phase shall be selected based on the method selected and the composition shall be finalized based on the interference of the blank peak and retention time i.e., which gives the least retention time without any interference.

5.4 Selection of Flow rate:

Select the flow rate, which gives the least retention time, good peak symmetries, less Back pressure and better separation from the blank peak.

5.5 Selection of Swab:

Select a swab (like Johnson swab, Texwipe swab etc.) which gives no interference with the analyte peak.

5.6 Selection of Diluent: Diluent for test preparation shall be selected initially based on solubility of the drug Substance. However, finalization of diluent shall be based on the satisfactory extraction efficiency for drug peak.

5.7 Selection of Injection volume:

Injection volume shall be selected based on the peak symmetries and response of the analyte peak

5.8 Swab interference:

Swab interference shall be checked after finalizing the entire method parameters for the particular drug substance.

5.9 Sonication time

Sonication time which gives the desired recovery of the Analyte shall be selected. Then the sonication time shall be altered by ±5 minutes and the effect of variation shall be checked.

After reviewing the results, the sonication time which is rugged for at least ±5 minutes shall be selected.

5.10 Filter Interference

Filter interference shall be checked with different types (at least 2 types) of filters after finalizing the entire method parameters for the particular drug substance.

Note: Swabbing experiments to optimize the recovery of Analyte in presence of excipients shall be carried out based on the requirement