SOP For FTIR - Pharmaceutical Guidelines

Standard Operating Procedure (SOP) for Operation, Calibration, Cleaning, and Maintenance of FTIR (Fourier Transform Infrared Spectrometer).

Table of Contents

Procedure for Operation and Calibration of FTIR

1.0 PURPOSE:

The purpose of this Standard Operating Procedure (SOP) is to describe the start-up, operation, calibration, and maintenance procedure of the FTIR – Fourier Transform Infrared Spectrophotometer.

2.0 SCOPE:

This SOP is applicable to the Shimadzu make and model IRAffinity-1 FTIR- Fourier Transform Infrared Spectrometer of the quality control department at the pharmaceutical drug manufacturing plant.

3.0 REFERENCES:

Instrument manual of Fourier Transform Infrared Spectrophotometer (FTIR).

SOP for Handling of out of Calibration results (OOC)

SOP for Analytical Instrument Qualification.

European Pharmacopoeia

SOP for -Instrument/Equipment usage log book.

SOP for –Maintenance of Laboratory Instruments.

4.0 RESPONSIBILITY & ABBREVIATIONS

The Analyst shall be responsible for the operate the instrument as per SOP,

Calibrate the instrument as per SOP and Recording all the document related to the operation, calibration, and maintenance.

Quality Control Head or Designee shall be responsible for give training to all the concerned persons before the implementation of SOP,

To ensure proper documentation as per SOP and initiate the maintenance activity white breakdown.

QA shall be responsible for check and ensure the implementation of the system as per SOP.

Quality Head and Plant Head shall be responsible for the review, approve the SOP.

ABBREVIATIONS:

FTIR: Fourier Transform Infrared Spectrophotometer.

KBr: Potassium Bromide

NA: Not Applicable

QA: Quality Assurance

QC: Quality Control

SOP: Standard Operating Procedure

4.0 PROCEDURE FOR OPERATION AND CALIBRATION OF FTIR:

Startup of FTIR Software

Clean the Instrument and surroundings.

Connect the instrument with the power supply.

Switch on the instrument and Computer system.

Double click on “IR Solution” Icon.

After No. of internal operation.

Select the “Measure” and select Measurement from the main menu, further select “ initialize” from the measurement tab.

Press “Yes” then following screen will appear:

Select File to load standard method for analysis or fill the desired parameter of the method.

Click on file,

Select the above option to enter the main window and select the standard method for analysis or prepare new method as per STP.

After selecting the standard method, double click on method or Open it from main window. A dialog box will appear and ask about downloading parameter of Method.

Press “OK” to download the method parameters

After completion of method downloading,

Click on “BKG” for background correction. A dialog box will appear.

Press “OK” if the Sample compartment is ready for Background.

Select measure from the above screen window, fill all the required (sample/standards information) in comment/Date file and select sample for sample analysis.

For the Sample Analysis click on the Data path file and give the appropriate file path for saving the data.

Copy the file name and paste the data in the comment and click on the sample tab.

After scanning the sample click on “Calculate” and then “OK” on the Peak Table.

The number of peaks in the Peak Table must be between 15 to 25.

To adjust the number of peaks click on “Calculate” and then increase or decrease the “Min Area” and then click on “OK”.

Click on “Window” from the main menu bar and select “Join Visible”.

Then click on “Manupulation 2” and select Purity.

Rightclick on the sample and select send to source similarly right click on the reference and select send to reference.
Send to reference

Click on “Calc”, then “OK”, select the print command from the main window.

Click on “OK” and select the desired report template for the Peak purity Graph as shown bellow.

Select the Report format and click on “Open” or double click on Report format. Press ‘OK’ for printing the document.

For Peak table : select the Manipulation 1 and select Peak table.

After selecting the peak table,

Click on “Calc” then “OK”.

Select “Print” from the above screen.

Select the report format as ‘peak table’ and print. As per the above described procedure.

Sample Preparation for FTIR Analysis:

Sample Preparation for solid Sample for FTIR Spectrometer:

Dry the KBr (Potassium Bromide –IR Spectroscopy grade) at 105°c for about 1 hour, cool it in the desiccator before use.

Crush the dried KBr in mortar.

Clean the sample holder with carbon tetrachloride or acetone to remove grease.

Take crushed KBr in the “Sample Cup” and plain the surface by using sample-pressing bar.

Clean the excess powder that fall on the sides of the sample cup using a tissue paper and put the cup on “Sample Cup Holder” in the sample compartment of the instrument.

Take the background IR.

Weigh about 300 mg of previously dried KBr and transfer it to a clean mortar.

Weigh about 2 to 4 mg of previously dried sample or as per the specified specification (to make sample concentration about 1.0% w/w) and transfer to the mortar, which contained the KBr.

Mix the sample with KBr for homogeneous.

Use this sample for the sample spectrum.

Sample preparation (For Liquid sample) for FTIR Spectrometer:

Select fixed thickness cell as per the requirement or use sodium chloride cell.

Put the cell in cassette and take the background (Air background) or as per the requirement.

Suck up the liquid sample by syringe.

Inject the liquid sample into the cell through the one hole of cell until the liquid came out from another hole of cell and become a thin film and insert the plugin both the holes.

Clean the cell with tissue paper.

Use this sample for sample spectrum.

Sample Preparations – Films.

Use this technique for liquids or semisolids or low melting solids.

Put the cell in cassette and take the background (Air background) or as per the

A thin film can be made by dissolving a semisolid or a highly viscous liquid (such as polymers) in a minimum volume of a volatile solvent (such as chloroform, carbon tetrachloride) or the sample can be taken as such.

Using a clean glass capillary, place a drop or a small portion of the sample onto a clean sodium chloride cell.

Hold the other sodium chloride cell’s edge on the top of the sample and slide horizontally applying slight pressure so as to form a thin film on the cell.

In case film is to be made with a solution, evaporate the solvent to dryness using a hot air gun. Align the cell edges and assemble the two sodium chloride cells.

Run a Background Scan as an air blank

Cut the film cassette size and insert a cassette.

Use this sample for the sample spectrum.

If the sample preparation is specified in the STP/ATP or individuals monograph follow the same.

Calibration (Verification of the wave-number scale) of FTIR Spectrometer:

Follow the operational procedure and record the Spectrum of the Polystyrene film over the range of 3800 cm^-1 to 650 cm^-1.

Record the wave number in attachment no. 01.

The spectrum should show the Transmission minima (absorption maxima) at the wave-number given in the attachment no. 01.

Frequency: (Monthly± 3 days)

Validation Procedure of FTIR Spectrometer:

Ensure that, the instrument is ready for calibration and the start-up procedure is followed.

Calibrate the instrument for power spectrum, resolution, wave number accuracy, repeatability of wave-number and repeatability of absorbance.

Ensure that the Instrument is ready for the calibration and start-up the procedure is followed.

Initialized the instrument.

Click on the icon Measurement, select “EP5.0 validation”.

After selecting “EP 5.0 validation”.

Click on “Measurement”.

Verify the necessary information or change the details as per requirements.

Click on “OK” to start the background.

After background validation completion,“ Set polystyrene film into the sample chamber” is displayed in the screen.

Set the polystyrene film accordingly and click on “OK”, scanning will start.

After completion of the validation the report will be generated and printed automatically.

Compare the results for its compliance against limits given in validation format and put remark regarding validation status.

Make entry of the usage into the Instrument usage logbook.

Calibration report shall come in form of validation format at the time of printing.( Annexure-2)

File the validation report duly signed and checked.

Affix calibration label on the instrument.

Frequency: Monthly ± 3 days

Precautions/Maintenance Program of FTIR Spectrometer:

Precautions during FTIR Calibration :

Use only spectroscopic grade KBr for the sample preparation and store a dry box.

Clean and dry mortar and pestle immediately after the usage.

Check silica bag of the dry box as well as sample compartment for its effectiveness.

When not in use Polystyrene film should be kept in its accompanying protective cover.

The exposed film surface should never be touched by fingers or any other objects and Dust should be removed by blowing with clean and dry air.

Breakdown Maintenance of FTIR Spectrometer :

Put “UNDER MAINTENANCE” label on the instrument when it is under breakdown maintenance / not functioning and intimate to Head quality or designer.

Head quality or desginee informs to the Instrument service engineer or Utility dept.

Keep instrument UNDER MAINTENANCE between breakdown and service period.

After maintenance, calibrate the instrument to check its satisfactory functioning and record the readings. (Note: Calibrate the instrument as per the calibration schedule, this calibration is additional)

Retain service report copy attached in the Instrument Maintenance History File.

5.0 ANNEXURES – SOP OF FTIR SPECTROMETER:

Annexure 1: FTIR Calibration Record.

Instrument Name: FTIR
Instrument No	Make/Model
Location	Calibration frequency	Monthly±3 days
Calibrated on	Next calibration due on

Sr.No	Date	Transmission minimum/absorption maximum (cm-1)	Observed wave number (cm-1)	Calibrated by	Checked by	Remarks
		3059-3061
	2848.5-2850.5
	1941.9-1943.9
	1600.2-1602.2
	1582.0-1584.0
	1153.5-1155.5
	1027.3-1029.3

Annexure 2: FTIR Validation Record.

Instrument Name: FTIR
Instrument No	Make/Model
Location	Calibration frequency	Monthly±3 days
Calibrated on	Next calibration due on

1. Power Spectrum	3. Wave Number Accuracy
Wave number	Measured	Standard Not less than	Wave number	Measured	Error	Tolerance
4600.0			3060.0			±1 cm-1
4000.0			2849.5			±1 cm-1
3000.0			1942.9			±1 cm-1
At maximum			1601.2			±1 cm-1
700.0			1583.0			±1 cm-1
500.0			1154.5			±1 cm-1
403.0			1028.3			±1 cm-1
351.0

2. Resolution	4. Repeatability of Wave Number
Wave number	Measured	Standard	Wave number	No.1	No.2	Error	Tolerance
Between 2870.0-2850.0		Greater than 0.33	2849.5				±5 cm-1
1601.2				±1 cm-1
Between 1589.0-1583.0		Greater than 0.08	1028.3				±1 cm-1

5.Repeatability of absorbance :
Wave number	No.1	No.2	Error	Tolerance
2849.5				±0.03%
1601.2				±0.05%
1028.3				±0.03%

Remark: The instrument is calibrated & qualified / Out of calibration & not qualified for use.

Calibration : Scheduled/Not scheduled (Reason : _________________________)

Done By: Date :

Checked By: Date :

Approved By: Date:

Annexure 3: Calibration Status label.

Quality Control

CALIBRATION STATUS

INSTRUMENT:

MAKE:

MODEL :

CALIBRATION ON :

CALIBRATION BY :

NEXT CALIBRATION DUE ON :