ANALYTICAL CLEANING METHOD VALIDATION

• OBJECTIVE:

To lay down the procedure for Validation of different types of analytical test procedures.

• SCOPE:

This SOP is applicable for the procedure for Validation of different types of analytical test procedures at {Company Name} {Location}.

• RESPONSIBILITY:
• Officer/Executive/Designee Quality Control – Shall be responsible for conducting validation of analytical test procedures as per SOP.
• Head/Designee Quality Control – Shall be responsible for ensuring compliance as per SOP.
• ACCOUNTABILITY:

             QA Head shall be Accountable for implementation of SOP.

• PROCEDURE:
  • All analytical methods shall be validated in accordance with current ICH Q1 requirements.
  • According to the current good manufacturing Practice Regulations [ (21CFR 211.194) (a) (2)], users of analytical methods described in (Compendial Method) are not required to validate accuracy and reliability of these methods, but merely to verify their suitability under actual conditions of use.
  • Analytical methods used for evaluation of cleaning process validation shall be done at Quality Control in accordance to the above guidelines.
  • Cleaning Validation Procedure:
    • Specificity:
      • Specificity is the ability to assess unequivocally the analyte in the presence of components which may be expected to be present.
      • Demonstrate the separation of the analyte from available placebo, Diluent, blank(swab) and placebo with standard solution using the Instrument.
    • System Precision:
      • The precision of an analytical procedure expresses the closeness of the agreement (Degree of scatter) between a series of measurements.
      • As a part of method validation, a minimum of 6 injections of the standard preparation with an RSD of ≤ 5.0 % is recommended.
    • Method Precision:
      • The precision of an analytical procedure expresses the closeness of the agreement (Degree of scatter) between a series of measurements obtained from a multiple sampling of the same homogeneous sample under the prescribed conditions.
      • As a part of method validation, a minimum of 6 injections of the standard preparation with an RSD of ≤ 5.0 % is recommended.
    • Linearity:
      • The linearity of an analytical procedure is its ability (with a given range) to obtain test results which are directly proportional to the concentration (amount) of analyte in the sample.
      • The Correlation coefficient should be greater than 0.99.
    • Limit of detection:
      • The limit of detection of an individual analytical procedure is the lowest amount of the analyte in a sample which can be detected but not necessarily quantified as an exact value.
      • Calculate LOD by using (3.3 x Steyx) / slope. Prepare and inject LOD solution accordingly. The % RSD should not be more than 33.0%.
    • Limit of Quantification:
      • The Quantification limit of an individual analytical procedure is the lowest amount of the analyte in a sample which can be quantitatively determined with a suitable precision and accuracy. The Quantification limit is a parameter of quantitative assays for low levels of compounds in sample matrices and is used particularly for the determination of impurities and/or degradation products.
      • Calculate LOQ by using (10 x Steyx) / slope. Prepare and inject LOQ solution (accordingly. The % RSD should not be more than 10.0 %.
    • Percentage Recovery:
      • Standard Solutions: Prepare standard solutions corresponding to approximately 50%, 100% and 150% of Acceptance Limit concentration as per the test procedure.
      • Spiked Swab solution: Prepare spiked swab solutions corresponding to approximately 50%, 100% and 150% of Acceptance Limit as per the test procedure.
      • Calculate the % Recovery of spiked swab using the following formula.

% Recovery = (Spiked swab Area / Average Standard Area) x 100

• Average % Recovery should be not less than 75%. In case of discrepancy repeat the experiment. If these criteria are still not met, investigate the reason.
  • Numbering of ACMV protocol and report:
    • Analytical Cleaning Method validation Protocol number consists of 15 characters.

ACMVP/QC/YY-XXX

where

ACMVP	:	Analytical Cleaning Method Validation protocol
/	:	slash
QC	:	Quality control
/	:	slash
YY	:	Current year
–	:	Dash
XXX	:	three digits serial number starts from 001,002 and so on

E.g.: First Analytical Cleaning Method Validation protocol of 2024 in QC shall be given as ACMVP/QC/24-001

• Analytical Cleaning Method validation Report numbering system consist of 15 characters

ACMVR/QC/YY-XXX

where

ACMVR	:	Analytical Cleaning Method Validation report
/	:	slash
QC	:	Quality control
/	:	slash
YY	:	Current year
–	:	Dash
XXX	:	three digits serial number starts from 001,002 and so on

E.g.: First Analytical Cleaning Method Validation report of 2024 in QC shall be given as ACMVR/QC/24-001.

• The Analytical Cleaning Method validation Protocol and Report along with supporting data shall be submitted to QA.

• REFERENCES:

Not Applicable

• ANNEXURES: 

ANNEXURE NO.	TITLE OF ANNEXURE
Annexure-I	Analytical Cleaning Method validation Record

      ENCLOSURES: SOP Training Record.

• DISTRIBUTION:
• Controlled Copy No. 01  :          Head Quality Assurance
• Controlled Copy No. 02  :         Head Quality Control
• Master Copy                    :          Quality Assurance Department
• ABBREVIATIONS:

No.	:	Number
HPLC	:	High Performance Liquid Chromatography
RSD	:	Relative standard deviation
SOP	:	Standard Operating Procedure
QC	:	Quality Control

• REVISION HISTORY:             

CHANGE HISTORY LOG

Revision No.	Details of Changes	Reason for Change	Effective Date
00	New SOP	Not Applicable	To Be Written Manual

Annexure-I
ANALYTICAL CLEANING METHOD VALIDATION LOGBOOK