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Standard Operating Procedure (SOP) for Operation and Calibration of FTIR Spectrophotometer used for identification test of starting material (RM) and drug product.

FTIR Spectrophotometer

1.0   Objective :

• • To lay down a procedure operation of FTIR Spectrophotometer. 

2.0   Scope :

• • This SOP is applicable for operation of FTIR Spectrophotometer (Make-BRUKER) in Quality Control Laboratory.

3.0   Procedure – Operation & Calibration of FTIR Spectrophotometer:  

• • Ensure that FTIR equipment is clean, if not clean, clean with soft cloth duster.

• • Check the calibration due date of FTIR.

• • System Check – FTIR:

• • Basic Module, which consist of low voltage air cooled IR Source, rock solid, Permanently adjusted Interferometer, ZnSe Beam Splitter, ZnSe window and Detector.

• • Exchangeable measurement module – ECO-ATR.

• • Computer with OPUS Software (Version 7.5.18).

• • Operation of FTIR System:

• • Confirm that the instrument is turned ‘ON’.

• • If the instrument is not turned ‘ON’ connect the plug to 230V stabilized power supply before switching on the instrument.

• • Locate the status light of the instrument; a green status light indicates the ready status of the instrument.

• • Switch ON the monitor & CPU.

• • Connect the basic module with an exchangeable measurement module depending on the physical property of the sample to be analysed.

• • Exchangeable measurement module ECO-ATR allows to spectroscopically analyse both solids (e.g. Paste & Powder).

• • To Exchange measurement module, press the lock on the basic module right down & pull out the measurement module from the basic module, push the new measurement module right against the basic module, press the lock on the basic module once again right down.

Note – The measurement module engages into the basic module and the lock snaps right up, OPUS will automatically recognize the measurement module. 

• • Log into the operating system by double clicking on ‘OPUS’ icon.

• • Enter appropriate ‘USER ID’ or select from the drop down list, enter ‘PASSWORD’ and click on ‘Login’ to start opus.

• • OPUS and ALPHA will communicate with each other and OPUS will start the ‘Performance test’ in the lower right corner a yellow message bubble appears informing that the performance test is running.

• • After successful completion of the test, the status light turns green.

• General measurement procedure can be subdivides into the following steps:

  • Basic Procedure of handling FTIR:

• • Click on measurement, select “Setup Measurement Parameters’.

• • Click on ‘Basic Tag’ in the cell provided for sample description,

• • Enter the current date, Sample/Product name, batch No._ test name and container ID number.

• • Click on ‘Advance’ tab, select appropriate path as select Drive E, current year and current month and save the file. For ex. – E\2021/Jan.

• • After all necessary variables are entered, click on ‘Save’ button to save the parameters method.

• • Click on ‘Accept’ & ‘Exit’.

• • To Add Sign on (ATR_ZnSe.XPM) Method:

• • Go to validation & select method- add signature / show history.

• • Select the desired method of (ATR_ZnSe.XPM) that has saved with parameters. Click on open.

• • Enter 21CFR user ID & password and click on OK.

• • Select option ‘Release’ and click on sign then close the file.

• • Now go to Advance Measurement click on background single channel.

• • After taking background put sample on ATR and click on sample single channel.

• • The standard spectrum will be saved.

• • Now to sign the standard spectra.

• • Go to validation and click on add signature.

• • Enter 21CFR user ID and password and click on OK.

• • Select option ‘Release’ and click on sign then close the window and unload the spectrum.

• • For taking sample spectra go to Advance Measurement and change the name in sample description,

• • Put sample on ATR and click on sample single channel and spectrum will be measured.

• • To sign the sample spectra go to validation and click on add signature.

• • Enter 21CFR11 user ID and Password and click on OK.

• • Select option ‘Release’ then click on sign and close the window.

• • Then click on unload for unload the file.

• • Now measure the standard and sample spectrum to make a comparison method which compares the sample spectrum with standard spectrum.

• • Go to evaluate and select quick compare setup.

• • Click on reference file and select the select single file. Select the single file and click on open then file will be added to it.

• • Click on parameter and select the threshold value 90 % then go to load/store method and click on store method.

• • Give the desired name of method and save then close the window by clicking on cross mark and unload the file.

• • To sign the method go to validation and select methods-add signature/show history then select the quick compare method (QCM) from list.

• • Click on Load method and open the desired method then click on add signature.

• • Enter 21CFR11 user ID and password then select the option release and click on sign then close the window.

• • To open the sample spectrums which will compare with saved standard method then go to file and click on load and open the sample spectrum file.

• • To evaluate and click on quick compare then click on load method and open the desired method. Click on compare.

• • After that a QC data block on upper side of spectrum on the graph. Double click on that then result will be shown.

• • Take the printout of results be clicking on quick print button then go to file and click on unload and close the software.

• • Preparing the Sample for FTIR Analysis:

  • When using exchangeable measurement module – ECO-ATR

• • Solid sample:

• • Clean the surface of crystal plate with integrated ATR Crystal with soft tissue.

• • Uniformly spread appropriate quantity of the sample on the ATR crystal.

• • Position the ‘Anvil’ over the sample and rotate the knob clock wise to press the anvil.

• • The sample is now ready to be scanned.

• • After scanning rotate the knob anticlockwise to release the anvil.

• • Clean the surface of crystal plate with integrated ATR crystal with soft tissue.

• • Liquid Sample:

• • Clean the surface of crystal plate with integrated ATR crystal with soft tissue.

• • Uniformly spread appropriate quantity of the sample on the ATR crystal.

• • The sample is now ready to be scanned.

• • After scanning clean the surface of crystal plate with integrated ATR crystal with soft tissue.

• • Measuring the sample spectrum (FTIR)

• • In the dialog window, click start sample measurement button.

• • The sample measurement takes few seconds.

• • The measurement progress is shown in the lower status bar.

• • The acquired sample spectrum is displayed in the OPUS spectrum window.

• • Take out print, check, sign and keep in record.

• • Enters the details in Instrument log (Annexure I of SOP No. QC-042).

• • Switch off the equipment and clean it.

• Calibration of FTIR:

  • Verification of the wave-number scale:

• • Place the polystyrene film in sample slot.

• • Record the spectrum of standard polystyrene film between 950 and 4000 cm^-1.

• • Verify the wave number scale by using polystyrene film as per the standard value given below:

• • Save the spectra and take the print. Enclose the duly checked and signed spectra along with Annexure-I.

• • Compare the result with calibration polystyrene film.

• • Enter the details in Annexure I.

• • Control of Resolution Performance:

• • For Fourier – transform instruments, use suitable instrument resolution, by recording the spectrum of a polystyrene film approximately 35µm in thickness.

• • The deference between the absorbance at the absorption minimum at 2870 cm^-1 and the absorption maximum at 2849.5 cm^-1 is greater than 0.33.

• • The deference between the absorbance at the absorption minimum at 1589 cm^-1 and the absorption maximum at 1583 cm^-1  is greater than0.08.

• • Enter the details in Annexure I.

• • Auto validation

• • Click on validation and run the OVP test.

• • Test results should be PASS and enter the details in Annexure I.

• • Prepare the calibration tag and affix it on the equipment.

• • Enclose the old calibration tag with the record and don’t throw it.

• • If the variation is not within the specified tolerance limits:

• • Label the equipment with a tag, “OUT OF CALIBRATION”.

• • Inform the Department Head.

• • Do not use equipment until all errors are rectified. After rectification, again calibrate the equipment & record the observation.

• • Frequency of FTIR Calibration:

• • 3 Months ± 3 days

4.0   References

• • Chapter No. 2.4.6 of IP 2014

• • Appendix IIA of BP 2015

• • Chapter No. 197 of USP

• • SOP :  Status Labeling

Annexure – I    : Calibration Record of FTIR Spectrophotometer

Model No.:                                                                      Eq. No. :………………….

Details of Polystyrene calibration film: …………………………

Certificate No.: ……………………….                      Validity date: …………………

Date of Calibration: ………………….                      Frequency: 3 Months ± 3 days

• Verification of the wave-number scale:

• Control of Resolution Performance:

•  Auto Validation: Result obtained PASS / FAIL.

Remarks: The observed values comply / does not comply the acceptance criteria and the equipment can be / cannot be used for routine analysis.

Next calibration due date : ………………….. 

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