Tablets: SOP for FTIR Analysis of Excipients in Tablets – V 2.0

Standard Operating Procedure for FTIR Analysis of Excipients in Tablets

Department	Quality Control
SOP No.	SOP/TAB/106/2025
Supersedes	SOP/TAB/106/2022
Page No.	Page 1 of 7
Issue Date	01/03/2026
Effective Date	06/03/2026
Review Date	01/03/2027

1. Purpose

To define the procedure for performing Fourier Transform Infrared (FTIR) spectroscopy analysis of excipients in tablet formulations, ensuring that the excipients used are accurately identified and meet the required quality standards.

2. Scope

This SOP applies to the FTIR analysis of excipients used in the manufacturing of tablets. It is used to confirm the identity and purity of excipients and ensure that they comply with specifications.

3. Responsibilities

Quality Control (QC): Responsible for performing FTIR analysis of excipients and ensuring that the results are within the required specifications.
Quality Assurance (QA): Ensures that the FTIR analysis procedure is followed correctly and reviews the results for compliance with regulatory standards and internal quality specifications.
Laboratory Personnel: Responsible for preparing samples, operating the FTIR instrument, and recording the results accurately.

4. Accountability

The QC Manager is accountable for ensuring that the FTIR analysis is performed accurately, and the results are interpreted according to established guidelines. The QA Manager is responsible for reviewing and approving the results before they are used in the production process.

5. Procedure

5.1 Sample Preparation

Weigh a representative sample of the excipient (usually 100 mg to 200 mg) from the batch for FTIR analysis.
Ensure that the sample is homogeneous and free from contamination.
For powdered excipients, mix with potassium bromide (KBr) at a ratio of 1:100, if required, and compress the mixture into a pellet using a hydraulic press. For liquids, no further preparation may be needed other than placing a few drops onto the FTIR sampling plate.
For tablets, crush the tablet and prepare a sample as described above.

5.2 FTIR Instrument Setup

Ensure that the FTIR instrument is calibrated and functioning correctly. Perform a background scan to check the instrument’s baseline.
Set the instrument parameters, such as the spectral range (typically 4000 cm^-1 to 400 cm^-1) and resolution (usually 4 cm^-1), according to the standard method or product specifications.
Prepare the FTIR sampling area, ensuring the sample holder is clean and free from residues.

5.3 Performing FTIR Analysis

Place the prepared sample in the FTIR instrument’s sample holder and initiate the analysis process.
Run the analysis, which will generate an infrared spectrum that corresponds to the molecular vibrations of the sample.
Ensure the scan is repeated several times (typically 16 scans) to obtain a high-quality spectrum.
Record the FTIR spectra for analysis and interpretation. Ensure that the spectrum is clear, with no overlapping peaks that could hinder the identification of the excipient.

5.4 Data Interpretation

Compare the obtained FTIR spectrum to the reference spectrum of the excipient to confirm its identity.
Check for characteristic peaks specific to the excipient. The absence or alteration of expected peaks may indicate contamination or improper formulation.
Evaluate the spectrum for any impurities or unidentified peaks that could affect the excipient’s quality and the final tablet formulation.
Document all relevant data, including sample preparation details, instrument settings, and the interpretation of the FTIR spectrum.

5.5 Acceptance Criteria

The FTIR spectrum should match the reference spectrum for the excipient with minimal deviation in peak positions and intensities.
Any significant differences between the sample spectrum and the reference spectrum must be investigated and documented in the deviation report (Annexure-1).
If the spectrum does not meet the expected criteria, initiate corrective actions, which may include re-analysis, additional testing, or sourcing a new excipient batch.

5.6 Documentation and Record-Keeping

Document all FTIR analysis results, including the spectra obtained, sample identification, and the comparison with reference spectra, in the batch record (Annexure-2).
Ensure that all records are signed, dated, and stored according to the company’s record retention policy for future audits and inspections.
Maintain raw data, including FTIR spectra and calibration data, for regulatory compliance and future reference.

5.7 Post-Test Actions

Clean the FTIR sampling area and the sample holder after each use to avoid cross-contamination between tests.
Dispose of any sample material and reagents according to the company’s waste disposal procedures.
Ensure that the FTIR instrument is maintained and calibrated according to the instrument’s SOP to ensure accurate results for future analyses.

6. Abbreviations

SOP: Standard Operating Procedure
GMP: Good Manufacturing Practice
QC: Quality Control
QA: Quality Assurance
FTIR: Fourier Transform Infrared
API: Active Pharmaceutical Ingredient

7. Documents

Batch Record (Annexure-2)
Deviation Report (Annexure-1)

8. References

USP <1970> – Infrared Spectroscopy for Pharmaceutical Analysis
21 CFR Part 211 – Current Good Manufacturing Practice for Finished Pharmaceuticals (US FDA)
European Pharmacopoeia (EP) – FTIR Analysis Specifications

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Deviation Report

Deviation Date	Batch Number	Deviation Description	Corrective Action	Responsible Person
15/12/2025	Batch 001	FTIR pattern did not match reference	Reanalyzed with new sample	John Doe

Annexure-2: Batch Record

Batch Number	Excipient	FTIR Spectrum ID	Comparison with Reference Spectrum	Result
Batch 001	Excipient X	XRDSpectrum_001	Match with Reference	Pass

Revision History:

Revision Date	Revision No.	Revision Details	Reason for Revision	Approved By
01/01/2024	1.0	Initial Version	New SOP Creation	QA Head
01/02/2025	2.0	Updated Analysis Procedure	Refined FTIR method	QA Head