Calibration of UV-Vis Spectrophotometer With Operation & Cleaning

SOPs

Calibration of UV-Vis Spectrophotometer Purpose :

Calibration of UV-Vis Spectrophotometer, The purpose of this SOP is to describe the operation, calibration and cleaning of UV-Vis Spectrophotometer (Shimadzu, UV-1800) used in the quality control laboratory of General block at XX Pharmaceuticals Limited.

Scope :

This procedure is applicable for UV-Vis Spectrophotometer (Shimadzu, UV-1800), installed in the quality control laboratory of XX Pharmaceuticals Limited.

Definitions / Abbreviation:

[][]SOP: Standard Operating Procedure.
[][]QC: Quality Control.
[][]UV-Vis: Ultraviolet and Visible.

Responsibilities:

Sr. Executive/Executive, QC

[][]To ensure that this procedure is followed.
[][]To maintain the records properly as per SOP.

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]To arrange training on the SOP to all concerned personnel and to ensure implementation of the SOP after training.
[][]Schedule calibration of the instrument at the defined intervals.

Head of Quality Assurance

[][]To ensure the overall implementation of the SOP.
[][]Approval of the SOP

Procedure:

Precaution(s):

[][]Prior to use, user must ensure that equipment is calibrated.
[][]Handle the measuring cell with care.
[][]Do not forget to turn off the instrument after use or if the next reading will be taken after long period of time.

Operation: Calibration of UV-Vis Spectrophotometer

[][]Switch ‘ON’ the Computer, Printer and Spectrophotometer.
[][]Wait until initialization is completed and the initialization result will be displayed in the outlet screen of the machine, finally green signal will appear in the outlet light-bar.
[][]Double click on ‘UV probe’ icon in the computer to run the software.
[][]Press ‘Connect’ icon to establish communications with the machine and machine will be ready for any type of analysis in Photometric/ Spectrum mode.

Measurement in spectrum mode

[][]Click “Spectrum” icon to perform measurement in spectrum mode.
[][]Click “Method” icon to set the desired parameters according to the requirement as follows:
[][]Click ‘Measurement’ icon then set following steps:
[][]Wavelength Range: Start & End- as required.
[][]Scan Speed : Fast/ Medium/ Slow/ Very slow
[][]Sampling Interval : As required
[][]Scan mode: Single/ Auto
[][]Input desired filename for the respective data to preserve in distinguishable data-path.
[][]Click ‘Instrument parameter’ to set the measuring mode as: Absorbance or transmittance.
[][]Finally press “OK” to resolve the setup, click ‘Close’.
[][]Click ‘ Baseline’ icon followed by ‘OK’ for baseline correction.
[][]Rinse both the cells with respective blank solution & wipe properly the outer surface of the cell with tissue paper. Put the cells in cell holder and close the curvature.

[][]Click “Auto zero” to compensate the blank reading.
[][]Remove one cell (front side) and after proper rinsing with the required sample solutions fill the cell with sample solution, wipe properly the outer surface of the cell with tissue paper & Set sample in the cell holder and finally close the curvature.
[][]Click “START”. The photometer status window will show “Slewing….” and it will be followed by the active reading.
[][]After completion of measurement click ‘Point pick’ for determining the absorbance/ transmittance at definite wavelength or Click ‘Peak pick’ for determining the absorbance/ transmittance at a given wavelength range.
[][]Click ‘Save’ to preserve the data and print the data on respective report format.
[][]Wash the measuring cells properly with purified water and preserve in appropriate place.

Measurement in quantitative mode

[][]Click “Photometric” icon to perform measurement in quantitative mode.
[][]Click “Method” icon to set the desired parameters according to the requirement as follows:
[][]Wavelength type: point
[][]Input required wavelength in ‘Wavelength (nm)’, click ‘Add’ then press Next
[][]Input ‘Type’ as ‘Single point’, Formula as ‘Fixed Wavelength’. In ‘WL1’ activate the required wavelength, then input standard concentration in ‘STD Concentration’, click Next>Next>Next.
[][]Finally in ‘Photometric method’ input ‘filename’ for the respective data to preserve in distinguishable data-path. Also input ‘Title’ if any, user name in ‘Analyst’ and fill-up ‘Comments’ if any.
[][]Press “Finish” to resolve the setup, click ‘Close’.
[][]Rinse both the cells with respective blank solution &swipe properly the outer surface of the cell with tissue paper. Put the cells in cell holder and close the curvature.

[][]Click “Autozero” to compensate the blank reading.

[][]Remove one cell (front side) and after proper rinsing with the required standard solutions fill the cell with standard solution, wipe properly the outer surface of the cell with tissue paper & Set standard solution in the cell holder and finally close the curvature.
[][]In the ‘Standard table’ input the standard description in the column for ‘Sample ID’, Click on ‘WL column’ and finally click ‘Read Std’ icon to measure the result.
[][]Remove the standard solution cell (front side) and after proper rinsing with the required sample solutions fill the cell with sample solution, wipe properly the outer surface of the cell with tissue paper & Set sample in the cell holder and finally close the curvature.
[][]In the ‘Sample table’ input the sample description in the column for ‘Sample ID’, Click on ‘WL column’ and finally click ‘Read Unk.’ icon to measure the result.
[][]Click ‘Save’ to preserve the data and print the data on respective report format.
[][]Wash the measuring cells properly with purified water and preserve in appropriate place.
[][]Click ‘Disconnect’ icon to detach the software from the machine.
[][]Exit from the ‘UV probe’ software by closing the window. Put off the power of equipment, printer and computer.

Calibration of UV-Vis Spectrophotometer:

[][]Calibrate the UV-Vis Spectrophotometer at 6 month’s frequency either by following procedure or as per supplier’s protocol:

Wave length Scanning

[][]Set desired start wavelength i.e. higher end of the desired spectrum and desired wavelength expansion. Scan the desired wavelength.

Control of Wavelengths

[][]Verify the wavelength at 241.15 nm, 287.15 nm, 361.5 nm & 536.3 nm using the absorption maximum of Holmium perchlorate solution (4% w/v solution of holmium oxide in a solution of perchloric acid containing 14.1% w/v of HClO4). The permitted tolerance is ± 1 nm for the ultraviolet range and ± 3 nm for the visible range. Record data in calibration information sheet as per Annexure-I .

Control of Absorbance

[][]Check the absorbance using a solution of potassium dichromate at the wavelengths indicated in (Annexure-I) which gives for each wavelength the exact values and the permitted limits of the specific absorbance. The tolerance for the absorbance is ± 0.01.
[][]For the control of absorbance, use solutions of potassium dichromate which has previously been dried to a constant mass at 130° C. For the control of absorbance at 235 nm, 257 nm, 313 nm and 350 nm, dissolve 57.0-63.0 mg of potassium dichromate in 0.005 M Sulphuric acid and dilute to 1000.0 ml with the same acid. For the control of absorbance at 430 nm, dissolve 57.0-63.0 mg of potassium dichromate in 0.005 M sulphuric acid and dilute to 100.0 ml with the same acid.
[][]Measure at a path length of 1 cm, at the wavelength 235 nm, 257 nm, 313 nm, 350 nm and 430 nm against 0.005 M Sulphuric acid as blank. Record data in calibration information sheet as per Annexure-I.

Limit of Stray light

[][]Detect stray light at a given wavelength with suitable solutions: for example the absorbance of a 12 g/l solution of potassium chloride in a 1 cm cell increases steeply between 220 nm and 200 nm and is greater than 2.0 at 198 nm when compared with water as compensation liquid. Record data in calibration information sheet as per Annexure-II.

Resolution (for qualitative analysis)

[][]Prepare a 0.02% v/v solution of toluene in hexane. Use hexane as a blank. The minimum ratio of the absorbance at the maximum at 269 nm to that at the minimum at 266 nm is not less than 1.5 unless otherwise stated in the monograph. Suitable certified reference materials may also be used. Record data in calibration information sheet as per Annexure-II.

Path length measurement of cell

[][]The tolerance on the path length of the cells used is ± 0.005 cm. When filled with the same solvent, the cells intended to contain the solution to be examined and the compensation liquid must have the same transmittance. If this is not the case, an appropriate correction must be applied.
The cells must be cleaned and handled with care.
[][]Carryout the test once before first use of a new cell.
[][]Affix the label “CALIBRATED “on the equipment if all results are satisfactory. If the equipment found out of calibration limit affix “NOT FIT FOR USE” label and call Supplier.

Cleaning procedure: Calibration of UV-Vis Spectrophotometer

[][]After completion of each analysis, clean the UV-Vis spectrophotometer as follows:
[][]Remove cuvette from the sample compartment.
[][]Remove the solution from the cuvette and wash with respective solvent in which solution is prepared.
[][]Rinse with water and then with methanol and wipe with tissue paper.
[][]Air dry and keep it at dedicated place.
[][]When required, clean the outer surface of the instrument with Isopropyl alcohol and dry it with tissue
paper.

Annexure:

Annexure-I: Calibration Information Sheet for UV-Vis Spectrophotometer (Control of Wavelength and Control of Absorbance)
Annexure-II: Calibration Information Sheet for UV-Vis Spectrophotometer (Resolution, Limit of Stray light)
Annexure-III: Operation Logbook for UV-Vis Spectrophotometer

 

 

 

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Calibration of FTIR Spectrophotometer with Cleaning and Operation

Quality Control, SOPs

Calibration of FTIR, Purpose:

Calibration of FTIR, The purpose of this SOP is to describe the operation, calibration and cleaning of FTIR Spectrophotometer (Shimadzu, IR Affinity-1) used in the quality control laboratory at XX Pharmaceuticals Limited.

Scope

This procedure is applicable for FTIR Spectrophotometer (Shimadzu, IR Affinity-1), installed in the quality control laboratory of XX Pharmaceuticals Limited.

Definitions / Abbreviation:

Standard Operating Procedure (SOP): Standard Operating Procedure. A written authorized procedure, which gives instructions for performing operations.

[][]QC: Quality Control.

[][]FTIR: Fourier Transform Infrared.

Responsibilities

[][]Executive/ Sr. Executive, QC

[][]To ensure that this procedure is followed.

[][]To maintain the records properly as per SOP

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]To arrange training on the SOP to all concerned personnel and to ensure implementation of the SOP after training.
[][]Schedule calibration of the instrument at the defined intervals.

Head of Quality Assurance

[][]Approval of the SOP.
[][]To ensure the overall implementation of the SOP.

Procedure: Calibration of FTIR

General Procedure:

[][]Ensure that the instrument is clean and calibrated.
[][]Connect the instrument properly with the power supply.
[][]Switch “ON” the main switch, power switch of the instrument situated at the backside panel, printer and computer.
[][]Allow the instrument initialize for at least 1 hour.

Disk preparation for solid sample:

[][]Mix 5 to 10 mg of sample with 200 to 400 mg of Potassium Bromide (KBr) [IR Grade].
[][]Grind the mixture to very fine powder with agate mortar.
[][]Pour the mixture into the barrel and carefully insert the plunger with its polished face downward.
[][]Maintain the hydraulic pressure 50 KN to 60 KN of the barrel for 1-2 minutes.
[][]Release the pressure and take out the disk from the barrel.
[][]For sample of liquid material using sealed liquid cell:
[][]Inject the liquid sample (pure or in solution) in sealed liquid cell.
[][]Plug to close both the slots of sealed liquid cell.
[][]For sample of liquid material which converted to solid (Nujol preparation) and measurement using NaCl demountable liquid cell:
[][]Put the cell window on the cell window holder and place the spacer of appropriate thickness on the cell window.
[][]Take 3 to 5 mg of sample with 2 to 3 drop of Nujol in a mortar and mix properly.
[][]Insert sample inside the spacer with a spatula. Put another cell window on the spacer and fit the metal plate on it.
[][]Fasten those plates with the four screws. Do not fix them with excessive force. It is enough to fasten them tightly by hand.

Operation Procedure (FTIR): calibration of FTIR

[][]Double click on “IRsolution” software icon.
[][]Press Measure
[][]Select FTIR Parameters in parameter window as follows:
[][]Data :
[][]Measurement Mode: % Transmitance ,
[][]Resolution: 2
[][]Apodization: Happ-Genzel
[][]No of Scans: 10
[][]Range (cm-1): Min: 400 cm-1 Max: 4000 cm-1
[][]Instrument:
[][]Beam: Internal
[][]Detector: Standard
[][]Mirror speed: 2.8
[][]More:
[][]Mode: Power
[][]Remove sample, if any, from the sample compartment.
[][]Click on Measurement then “Initialize” then “Yes”.

[][]After successful initialization, click BKG then “OK”. Wait till window on the screen is displayed as last Bkg.
[][]After ‘Bkg scan’, put the sample disk in the sample chamber, with the help of sample holder and close the chamber.
[][]Enter the Sample name, Batch No., Sample ID. in comment box and enter the data file location in Data file box.
[][]Click Sample to measure sample. Wait till the actual sample IR scan is displayed.
[][]Click on the spectrum window. Select Calculate  peak table. Type threshold: 60.00.
[][]Click on Calc, OK
[][]Compare the Spectrum in computer screen. View the IR scan of standard, click on Manipulation 2 then “Purity” then “Yes”.
[][]Again view the IR scan of sample, click on Manipulation 2  “Purity”  “Calc”  “OK”.
[][]After comparison with standard and sample then click file and open file as required. Then click Window  “Join visible”  “Calc”  “OK”.
[][]Purity index should be within 0 .9500 – 1.0000.
[][]A disc is rejected if visual examination shows lack of uniform transparency or when transmittance at about 2000 cm-1 (5 µm) in the absence of a specific absorption band is less than 60 % without compensation, unless otherwise prescribed in individual monograph.
[][]For printing of spectrum, click File  “Print preview”. Select respective necessary template and then print.
[][]Close the parameter window and the Software window.
[][]Shutdown PC, switch off Printer.
[][]Power OFF Spectrophotometer.
[][]Take out the liquid cell from the instrument.
[][]Discard the disk /Nujol / liquid sample.
[][]Clean the holder and liquid cell with dry and clean tissue paper.
[][]In case of sealed liquid cell mop and wash with IPA or absolute Ethanol and in case of demountable liquid cell mop and wash with Chloroform or Carbon Tetrachloride.
[][]Keep them in specified desiccator.
[][]Rub mortar, pestle, barrel & plunger with tissue paper to make them free from dust.
[][]Mop them with a tissue paper soaked in absolute ethanol.
[][]Keep them in a desiccator for next operation.
[][]Record all analysis in operation log book as per Annexure-II.

Operation Procedure (ATR):

Running a sample:

[][]Turn on the computer and crick on the respective software on the desktop.
[][]Set the MIRacle/ MIRacle A Base Unit to the instrument.
[][]Before initialization, set FTIR Parameters in parameter window as follows:
[][]Data :
[][]Measurement Mode: % Transmitance ,
[][]Resolution:2
[][]Apodization: Happ-Genzel
[][]No of Scans: 10
[][]Range (cm-1): Min : 700 cm-1 Max : 4000 cm-1
[][]Click on Measurement then “Initialize” then “Yes”. Click “cancel” option for auto adjustment.
[][]Click on Measurement then “Auto adjustment (Fine)” then “Yes”.
[][]After autoadjustment, click BKG then “OK”. Wait till window on the screen is displayed as last Bkg.
[][]Set the clamp to the base. Place sample on the ZnSe crystal- Liquids -place a drop of sample on the ZnSe crystal. Place a small neat solid sample on the ZnSe crystal with a spatula. Adjust the knob of the ATR until the pressure reads 12.
[][]Make sure that no acid sample (pH below 5), strong alkaline sample (pH more than 9) or liquid which give damage to PTFE should not be place on ZnSe prism.
[][]Enter the Sample name, Batch No., Sample ID. in comment box and enter the data file location in Data file box. Click Sample to measure sample. Wait till the actual sample ATR scan is displayed.

Working up the Data:

[][]Compare the Spectrum in computer screen. View the ATR scan of standard, click on Manipulation 2 then “Purity” then “Yes”.
[][]Again view the ATR scan of sample, click on Manipulation 2  “Purity”  “Calc”  “OK”.
[][]After comparison with standard and sample then click file and open file as required. Then click Window  “Join visible”  “Calc”  “OK”.
[][]For printing of spectrum, click File  “Print preview”. Select respective necessary template and then print

Calibration:

[][]Calibrate the FTIR Spectrophotometer at 6 month’s frequency either by following procedure or as per supplier’s protocol:
[][]Power ON the Spectrometer. Wait for at least 1 hour. Power ON PC & Printer.
[][]Double click on “IRsolution” software icon. Press Measure
[][]Select FTIR Parameters in parameter window as follows:
[][]Data :
[][]Measurement Mode: % Transmitance ,
[][]Resolution : 2
[][]Apodization : Happ-Genzel
[][]No of Scans : 10
[][]Range (cm-1) : Min : 400 cm-1 Max : 4000 cm-1
[][]Instrument :
[][]Beam : Internal
[][]Detector : Standard
[][]Mirror speed : 2.8
[][]More :
[][]Mode : Power
[][]Remove sample, if any, from the sample compartment.
[][]Click on Measurement then “Initialize” then “Yes”.
[][]After successful initialization, click BKG then “OK”. Wait till window on the screen is displayed as last Bkg.
[][]After ‘Bkg scan’, place the Polystyrene film in the sample chamber and close the chamber.
[][]Enter the Polystyrene 1 and Wave number verification in comment box and enter the data file location in Data file box.
[][]Click Sample to scan the polystyrene film (0.05 mm thick). Wait till the actual sample IR scan is displayed.
[][]Click on the spectrum window. Select Calculate  peak table. Type threshold: 65.00.
[][]Click on Calc  OK
[][]For printing of spectrum, click File  “Print preview”. Select respective necessary template and then print. Collect Polystyrene spectrum and peak table printed in two pages.

Limit of Wave Number Accuracy

[][]Check the maximum at following wave numbers (cm-1): 3060.0 (±1.5) cm-1, 2849.5 (±1.5) cm-1, 1942.9 (±1.5) cm-1, 1601.2 (±1.0) cm-1, 1583.0 (±1.0) cm-1, 1154.5 (±1.0) cm-1, 1028.3 (±1.0) cm-1.
[][]Resolution of apparatus
[][]Resolution due to transmittance:
[][]Record the Spectrum of a polystyrene film of approximately 35 µm thickness using Measuring Mode: % T.
[][]Measure the percentage transmittance at the transmission maximum at 2870 cm-1 (3.48 µm) and that at the transmission minimum at 2849.5 cm-1 (3.51 µm).
[][]Measure the percentage transmittance at the transmission maximum at 1589 cm-1 (6.29 µm) and that at the transmission minimum at 1583 cm-1 (6.32 µm).
[][]Record the results in calibration information sheet as per Annexure-I.

Acceptance criteria:

[][]The difference between the % transmittance at the transmission maximum at 2870 cm-1 (3.48 µm) and that at the transmission minimum at 2849.5 cm-1 (3.51 µm) must be greater than 18.
[][]The difference between the percentage transmittance at the transmission maximum at 1589 cm-1 (6.29 µm) and that at the transmission minimum at 1583 cm-1 (6.32 µm) must be greater than 10.

Resolution due to Absorbance:

[][]Record the Spectrum of a polystyrene film of approximately 35 µm thickness using Measuring Mode: Abs.
[][]Measure the absorbance at the absorption minimum at 2870 cm-1 and the absorption maximum at 2849.5 cm-1.
[][]Measure the absorbance at the absorption minimum at 1589 cm-1 and the absorption maximum at 1583 cm-1.
[][]Record the results in calibration information sheet as per Annexure-I.

Acceptance criteria:

[][]The difference 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 difference between the absorbance at the absorption minimum at 1589 cm-1 and the absorption maximum at 1583 cm-1 is greater than 0.08.
[][]If the calibration is not within the specified standards, check the cleanliness of polystyrene film again and repeat the calibration.
Wavelength Repeatability Test:
[][]Repeat the Spectrum of the polystyrene film and Superimposed one after another of the absorption bands at 2849.5 cm–1 (3.51 µm), 1601.2 cm–1 (6.25 µm), 1028.3 cm –1 (9.72 µm).
[][]Acceptance Criteria: Compare the difference within 0.5% of the wave number scale and Purity index should be within 0.9500 – 1.0000
[][]Affix the label “CALIBRATED “on the equipment if all results are satisfactory. If the equipment found out of calibration limit affix “NOT FIT FOR USE” label and inform supplier.

Cleaning procedure:

[][]Clean the instrument with clean dry cloth daily.
[][]Remove your sample from the ATR, by using a cloth that is damped with acetone.
[][]Clean the plunger in the same way, if it made contact with sample.
[][]Never squirt (spray) acetone directly on the platform.

Annexure: Calibration of FTIR

Annexure-I: Calibration Information Sheet for FTIR Spectrophotometer
Annexure-II: Operation Logbook for FTIR Spectrophotometer

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Electric Analytical Balance Calibration, Cleaning & Daily Accuracy Check

Quality Control, SOPs

Electric Analytical Balance Calibration; Purpose :

Electric Analytical Balance Calibration; The purpose of this SOP is to describe the operation, calibration, cleaning and daily accuracy check of Electric Analytical Balance

Scope :

This procedure is applicable for Electric Analytical Balance , installed in the quality control laboratory of XX Pharmaceuticals Limited.

Definitions / Abbreviation:

[][]SOP: Standard Operating Procedure
[][]QC: Quality Control

Responsibilities:

Executive/Sr. Executive, QC

[][]To ensure that this procedure is followed.
[][]To ensure daily accuracy check of the balances.
[][]To maintain the records properly as per SOP.
[][]To preserve calibration, daily accuracy check record.

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]Arrange training on the SOP to all concerned personnel.
[][]To ensure implementation of the SOP after training.

Head of Quality Assurance

[][]Approval of the SOP
[][]To ensure the overall implementation of the SOP.

Procedure:

General precautions:

[][]Do not move or replace Balance after calibration. If require, calibrate after movement.
[][]Do not place Balance near to heat generating equipment or direct sunlight.
[][]Clean up any spillage in or around the balance immediately after operations.
[][]Proper protective clothing such as safety glasses, gloves and Laboratory coat must be worn during weighing process.
[][]Do not use sharply pointed objects to operate the keyboard of balance.
[][]Do not use cleaning agents which contain solvents or abrasive ingredients.

Operation:

To start up:

[][]Level and adjust at each time it is moved to a new location. The balance is exactly horizontal when the air bubble is in the middle of the level glass. Adjust the two front leveling feet appropriately until the air bubble comes to rest exactly in the middle of the glass.
[][]Plug the AC adapter and connect the power supply. Connect the printer to the balance.
[][]Switch on the printer using I/O switch.
[][]Press On/Off () button to on the Electric Analytical Balance. Display will show 0.0000g.
[][]Convert the weighing unit from g into mg, press scroll down button if necessary.
[][]Allow the balance to warm up to enable it to adapt itself to the ambient condition.
[][]Long press for menu button and select ‘BASIC’ by single press Enter button
[][]Set date, time and unit using keys and Enter button and save the settings using button.
[][]Press cancel (C) button to return come out of that ‘BASIC’ option and return to its main menu

Weighing:

[][]Check the machine is clean and calibrated. Then remove all loads from weighing pan.
[][]When zero (0.0000 g) reading is displayed, the balance is ready for operation. If the display shows greater than or less than zero, press tare button to tare the balance.
[][]If the balance is not in the weighing mode, press and hold the key down until ‘WEIGHING’ in the display.
[][]Use handle/coupling element for the operation of the draft shield door of the both side of the instrument.
[][]Open right/left/upper sliding window of the instrument.
[][]Place empty container/weighing paper on the pan of the balance. Close the sliding window.
[][]The weight is displayed. Allow the reading to stabilize and wait until the instability detector disappears from the left side of the display and the stability beep sounds.
[][]Press Tare button to tare the balance. When zero (0.0000 g) reading is displayed, the balance is ready for weighing.
[][]The weighing-in aid is a dynamic graphic indicator which shows the used amount of the total weighing range. It can be recognized at a glance when the load on the balance approaches the maximum load.
[][]Add weighing sample (Maximum 120 g) on the container/weighing paper using weighing spoon. Close the sliding window. The net weight is now displayed.
[][]Allow the reading to stabilize and wait until the instability detector (O) disappears from the left side of the display and the stability beep sounds
[][]To get printout of the weight, press print button.
[][]For performing another weighing press Tare button to tare the balance and follow previous steps from to increase or decrease digit, press display resolution button.
[][]Finally, press and hold On/Off button button untill ‘SHUT OFF’ shows on the display.
[][]Fill up the Operation Log book for Semi-Micro Balance (as per Annexure-II).

Daily Accuracy Check:

[][]Perform the Internal and External Calibration as per below mentioned procedure
[][]Take 20 g, 70 g of certified weight and clean it with a soft cloth.
[][]Use tare button to tare the balance before start with a weighing.
[][]Always press button to tare the balance between the interval of one weight to another and observe whether the instability detector (O) disappears from the left side of the display or not and the balance will give a stability beep sounds.
[][]Open one sliding window and place the weights separately at the center of the weighing pan, close the sliding window and allow the reading to be stabilized and wait until the instability detector (O) disappear from the left side of the display and the stability beep sounds.
[][]Print the results by pressing print button if necessary.
[][]Record the value of those weights in Log Book for Daily Accuracy Check (as per Annexure-I).

Calibration:

Internal Calibration:
Manual Adjustment with Internal weight:

[][]Long press menu button and press scroll down button to go to ‘ADVANCED’ option.
[][]Select ‘ADVANCED’ by pressing Enter button.
[][]Press scroll down button once to select ‘CAL’ option by pressing Enter button.
[][]Then select ‘ADJ. INT’ using scroll down button and then press Enter button.
[][]Press Cancel (C) twice and save the settings if required by scrolling down button and press Enter button and then return to its main menu.
[][]Unload weighing pan Press and hold calibration button to execute ‘Internal Adjustment’.
[][]The balance adjusts itself automatically. The adjusting is finished when the message “ADJ.DONE” appears briefly on the display. The balance returns to the last active application and is ready for operation.
[][]After adjustment, the result of the calibration will be printed out automatically or press print (button for print copy.

External Calibration:

Manual Adjustment with External weight:

[][]Long press menu button and press scroll down button to go to ‘ADVANCED’ option.
[][]Select ‘ADVANCED’ by pressing Enter button.
[][]Press scroll down button once to select ‘CAL’ option by pressing Enter button.
[][]Select ‘ADJ. EXT’ by using scroll down and then press Enter button.
[][]Set the adjustment weight (100g) by using -/+ key for External Calibration and press Enter button.
[][]Then press cancel (C) button twice and save the settings if required by using -/+ key and press Enter button and then return to its main menu.
[][]Unload weighing pan Press and hold calibration button to execute ‘External Adjustment’.
[][]The required predefined adjustment weight value flashes on the display.
[][]Place adjustment certified weight on the center of pan. The balance adjusts itself automatically.
[][]When ‘0.0000 g’ flashes, remove the adjustment weight.
[][]The adjustment is finished when the message ‘ADJ DONE’ appears briefly on the display. The balance returns to the last active application and is ready for operation.
[][]After adjustment, the result of the calibration will be printed out automatically or press print button for print copy.

Eccentricity:

[][]Take 20 g, 70 g of certified weight and clean it with a soft cloth.
[][]Use tare button to tare the balance before start with a weighing.
[][]Always press button to tare the balance between the interval of one weight to another and observe whether the instability detector (O) disappears from the left side of the display or not and the balance will give a stability beep sounds.
[][]Place 50g weight at center, Left Rear, Right Rear, right Front, Left Front and center on the pan again separately.
[][]Allow the reading to be stabilized in each time while weighing and wait until the instability detector (O) disappear from the left side of the display and the stability beep sounds.
[][]Press print button separately to print each individual reading in same print page.

Linearity:

[][]Use Tare button to tare the balance before start with a weighing.
[][]Always press button to tare the balance between the interval of one weight to another and observe whether the instability detector (O) disappears from the left side of the display or not and the balance will give a stability beep sounds.
[][]Place 10 g, 20 g and 50 g on the center of pan separately.
[][]Allow the reading to be stabilized in each time while weighing and wait until the instability detector (O) disappear from the left side of the display and the stability beep sounds.
[][]Press Print ( ) button separately to print each individual reading in same print page.

Sensitivity:

[][]Use Tare button to tare the balance before start with a weighing.
[][]Always press button to tare the balance between the interval of one weight to another and observe whether the instability detector (O) disappears from the left side of the display or not and the balance will give a stability beep sounds.
[][]Place 100 g on the center of pan.
[][]Allow the reading to be stabilized in each time while weighing and wait until the instability detector (O) disappear from the left side of the display and the stability beep sounds.
[][]Press Print ( ) button separately to print each individual reading in same print page.

Repeatability:

[][]Use Tare button to tare the balance before start with a weighing.
[][]Always press button to tare the balance between the interval of one weight to another and observe whether the instability detector (O) disappears from the left side of the display or not and the balance will give a stability beep sounds.
[][]Place 100 g on the center of the pan for ten times separately.
[][]Allow the reading to be stabilized in each time while weighing and wait until the instability detector (O) disappear from the left side of the display and the stability beep sounds.
[][]Press Print ( ) button separately to print each individual reading in same print page.

Result:

[][]Record all the values for calibration in Calibration Information Sheet for Electric Analytical Balance (as per Annexure-III).
[][]Perform the Calibration of the Electric Analytical Balance once after every six months.

Cleaning:

[][]Ensure that no liquid comes into contact with the balance and AC adapter.
[][]Remove all objects from the balance.
[][]Clean the pan with soft brush followed by with soft clean cloth.
[][]Clean all of the parts of the balance with clean dry cloth.
[][]Set the parts of weighing pan carefully.

 

Annexure:

Annexure-I: Log book for Daily Accuracy Check of Electric Analytical Balance
Annexure-II: Operation Log book for Electric Analytical Balance
Annexure-II: Calibration Information Sheet for Electric Analytical Balance

Electric Analytical Balance Calibration, Cleaning & Daily Accuracy Check Read More »

Calibration of Semi-Micro Balance

Quality Control, SOPs

Calibration of Semi-Micro Balance; Purpose :

Calibration of Semi-Micro Balance; The purpose of this SOP is to describe the operation, calibration, cleaning and daily accuracy check of Semi-Micro Balance (Model: MS205DU).

Scope :

This procedure is applicable for Semi-Micro Balance (Model: MS205DU), installed in the quality control laboratory of XX Pharmaceuticals Limited.

Definitions / Abbreviation:

[][]SOP: Standard Operating Procedure
[][]QC: Quality Control

Responsibilities:

Executive/Sr. Executive, QC

[][]To ensure that this procedure is followed.
[][]To ensure daily accuracy check of the balances.
[][]To maintain the records properly as per SOP.
[][]To preserve calibration, daily accuracy check record.

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]Arrange training on the SOP to all concerned personnel.
[][]To ensure implementation of the SOP after training.

Head of Quality Assurance

[][]Approval of the SOP
[][]To ensure the overall implementation of the SOP.

Procedure:

General precautions:

[][]Do not move or replace Balance after calibration. If require, calibrate after movement.
[][]Do not place Balance near to heat generating equipment or direct sunlight.
[][]Clean up any spillage in or around the balance immediately after operations.
[][]Proper protective clothing such as safety glasses, gloves and Laboratory coat must be worn during weighing process.
[][]Do not use sharply pointed objects to operate the keyboard of balance.
[][]Do not use cleaning agents which contain solvents or abrasive ingredients.

Calibration of Semi-Micro Balance; Operation:

To start up:

[][]Level and adjust at each time it is moved to a new location. The balance is exactly horizontal when the air bubble is in the middle of the level glass. Adjust the two front leveling feet appropriately until the air bubble comes to rest exactly in the middle of the glass.

[][]Plug the AC adapter and connect the power supply. Connect the printer to the balance.
[][]Switch on the printer using I/O switch.

[][]Press On/Off button to on the Semi-Micro Balance. Display will show 0.00000 g.
[][]Convert the weighing unit from g into mg, press scroll down button if necessary.
[][]Allow the balance to warm up to enable it to adapt itself to the ambient condition.
[][]Press menu button and select ‘BASIC’ by pressing Enter button
[][]Set date, time and unit using -/+ keys and Enter button and save the settings.
[][]Press cancel (C) button to return come out of that ‘BASIC’ option and return to its main menu.
[][]Perform the daily accuracy check at the starting of the day.

Calibration of Semi-Micro Balance; Weighing:

[][]Check the machine is clean and calibrated. Then remove all loads from weighing pan.
[][]When zero (0.00000 g) reading is displayed, the balance is ready for operation. If the display shows greater than or less than zero, press Tare button to tare the balance.
[][]If the balance is not in the weighing mode, press and hold the key down until ‘WEIGHING’ in the display.
[][]Use handle/coupling element for the operation of the draft shield door of the both side of the instrument.
[][]Open right/left/upper sliding window of the instrument.
[][]Place empty container/weighing paper on the pan of the balance. Close the sliding window.
[][]The weight is displayed. Allow the reading to stabilize and wait until the instability detector (O) disappears from the left side of the display and the stability beep sounds.

[][]Press Tare button to tare the balance. When zero (0.00000 g) reading is displayed, the balance is ready for weighing.
[][]The weighing-in aid is a dynamic graphic indicator which shows the used amount of the total weighing range. It can be recognized at a glance when the load on the balance approaches the maximum load.
[][]Add weighing sample (Maximum 220 g) on the container/weighing paper using weighing spoon. Close the sliding window. The net weight is now displayed.
[][]Allow the reading to stabilize and wait until the instability detector disappears from the left side of the display and the stability beep sounds
[][]To get printout of the weight, press print button.

[][]For performing another weighing press tare (O/T) button to tare the balance and follow all steps described above. To increase or decrease digit, press display resolution button.

[][]Finally, press and hold On/Off button ( ) button until ‘SHUT OFF’ shows on the display.
[][]Fill up the Operation Log book for Semi-Micro Balance (as per Annexure-II).

Daily Accuracy Check:

[][]Perform the Internal and External Calibration as per below mention Steps under Calibration.
[][]Take 50 g, 150 g of certified weight and clean it with a soft cloth.
[][]Use tare button to tare the balance before start with a weighing.
[][]Always press button to tare the balance between the interval of one weight to another and observe whether the instability detector (O) disappears from the left side of the display or not and the balance will give a stability beep sounds.
[][]Open one sliding window and place the weights separately at the Centre of the weighing pan, close the sliding window and allow the reading to be stabilized and wait until the instability detector (O) disappear from the left side of the display and the stability beep sounds.
[][]Print the results by pressing print button if necessary.
[][]Record the value of those weights in Log Book for Daily Accuracy Check (as per Annexure-I).

Calibration:

Internal Calibration:

Manual Adjustment with Internal weight:

[][]Press menu button and then press scroll down to go to ‘ADVANCED’ option.
[][]Select ‘ADVANCED’ by pressing Enter button.
[][]Press scroll down button once to select ‘CAL’ option by pressing Enter button.
[][]Then select ‘ADJ. INT’ using scroll down button and then press Enter button.
[][]Press cancel (C) twice and save the settings if required by scrolling down button and press Enter button and then return to its main menu.
[][]Unload weighing pan Press and hold calibration button to execute ‘Internal Adjustment’.
[][]The balance adjusts itself automatically. The adjusting is finished when the message “ADJ.DONE” appears briefly on the display. The balance returns to the last active application and is ready for operation.
[][]After adjustment, the result of the calibration will be printed out automatically.

External Calibration:

Manual Adjustment with External weight:

[][]Follow the previous instruction[Manual Adjustment with Internal weight] for manual adjustment.
[][]Select ‘ADJ. EXT’ by using scroll down and then press Enter button.
[][]Enter the adjustment weight (200g) by using -/+ key for External Calibration and press Enter button.
[][]Then press cancel (C) button twice and save the settings if required by scrolling down button and press Enter button and then return to its main menu.
[][]Unload weighing pan Press and hold calibration button to execute ‘External Adjustment’.
[][]The required predefined adjustment weight value flashes on the display.
[][]Place adjustment certified weight on the center of pan. The balance adjusts itself automatically.
[][]When ‘0.0000 g’ flashes, remove the adjustment weight.
[][]The adjustment is finished when the message ‘ADJ DONE’ appears briefly on the display. The balance returns to the last active application and is ready for operation.

Eccentricity:

[][]Take 50 g, 150 g of certified weight and clean it with a soft cloth.
[][]Use Tare button to tare the balance before start with a weighing.
[][]Always Press button to tare the balance between the interval of one weight to another and observe whether the instability detector (O) disappears from the left side of the display or not and the balance will give a stability beep sounds.
[][]Place 100 g weight at center, Left Rear, Right Rear, right Front, Left Front and center on the pan again separately.
[][]Allow the reading to be stabilized in each time while weighing and wait until the instability detector disappear from the left side of the display and the stability beep sounds.
[][]Press print button separately to print each individual reading in same print page.

Linearity:

[][]Take 50 g, 150 g of certified weight and clean it with a soft cloth.
[][]Use tare button to tare the balance before start with a weighing.
[][]Always press button to tare the balance between the interval of one weight to another and observe whether the instability detector disappears from the left side of the display or not and the balance will give a stability beep sounds.
[][]Place 20 g, 50 g, 100 g, and 200 g on the center of pan separately.
[][]Allow the reading to be stabilized in each time while weighing and wait until the instability detector (O) disappear from the left side of the display and the stability beep sounds.
[][]Press Print button separately to print each individual reading in same print page.

Sensitivity

[][]Take 50 g, 150 g of certified weight and clean it with a soft cloth.
[][]Use tare button to tare the balance before start with a weighing.
[][]Always press button to tare the balance between the interval of one weight to another and observe whether the instability detector disappears from the left side of the display or not and the balance will give a stability beep sounds.
[][]Place 200 g on the center of pan.
[][]Allow the reading to be stabilized in each time while weighing and wait until the instability detector (O) disappear from the left side of the display and the stability beep sounds.
[][]Press Print button separately to print each individual reading in same print page.

Repeatability (200 g):

[][]Take 50 g, 150 g of certified weight and clean it with a soft cloth.
[][]Use tare button to tare the balance before start with a weighing.
[][]Always press button to tare the balance between the interval of one weight to another and observe whether the instability detector disappears from the left side of the display or not and the balance will give a stability beep sounds.
[][]Place 200 g on the center of the pan for ten times separately.
[][]Allow the reading to be stabilized in each time while weighing and wait until the instability detector (O) disappear from the left side of the display and the stability beep sounds.
[][]Press Print button separately to print each individual reading in same print page.

Repeatability (20 g):

[][]Take 50 g, 150 g of certified weight and clean it with a soft cloth.
[][]Use tare button to tare the balance before start with a weighing.
[][]Always press button to tare the balance between the interval of one weight to another and observe whether the instability detector disappears from the left side of the display or not and the balance will give a stability beep sounds.
[][]Place 20 g on the center of the pan for ten times separately.
[][]Allow the reading to be stabilized in each time while weighing and wait until the instability detector (O) disappear from the left side of the display and the stability beep sounds.
[][]Press Print button separately to print each individual reading in same print page.

Result:

[][]Record all the values for calibration in Calibration Information Sheet for Semi-Micro balance (as per Annexure-III).
[][]Perform the Calibration of the Semi-Micro Balance once in every six months.

Cleaning:

[][]Ensure that no liquid comes into contact with the balance and AC adapter.
[][]Remove all objects from the balance.
[][]Clean the pan with soft brush followed by with soft clean cloth.
[][]Clean all of the parts of the balance with clean dry cloth.
[][]Set the parts of weighing pan carefully.

Annexure:

Annexure-I: Log book for Daily Accuracy Check of Semi-Micro Balance
Annexure-II: Operation Log book for Semi-Micro Balance
Annexure-II: Calibration Information Sheet for Semi-Micro balance

Calibration of Semi-Micro Balance Read More »

Maintenance of Desiccator

Quality Control, SOPs

Maintenance of Desiccator; Purpose :

Maintenance of Desiccator; The purpose of this procedure is to describe the maintenance (handling and cleaning) of desiccator.

Scope :

This procedure is applicable for all desiccators in the quality control laboratory of XX Pharmaceuticals Ltd.

Definitions / Abbreviation:

Desiccant canister: A container with hygroscopic substance which induces or sustains a state of dryness in its area.

Responsibilities:

Officer/ Executive, QC

[][] To follow the instructions of this procedure correctly.

Sr. Executive, QC

[][] To ensure that SOP is followed correctly.

Manager, Quality Control

[][] To ensure that this procedure is kept up to date.
[][] To ensure appropriate personnel from the section are trained on this procedure.
[][] To confirm that SOP is technically sound and reflects the required working practices.

Manager, Quality Assurance

[][]Approval of the SOP.
[][]To ensure the overall implementation of the SOP.

Procedure:

Precaution(s):

[][]Do not touch hot samples, while transferring them from Oven/Muffle furnace to desiccator.

Operation

[][]Place about 200 g of silica (desiccant) and/or dessicant canister into the bottom of the desiccator.
[][]Set the sample platform (desiccator plate) to the desiccator.
[][]Apply a smear of grease in between lid & desiccator rim to avoid sticking of lid with the dessicator.
[][]Close the lid properly.
[][]Open the lid to retain the sample to be analyzed and close the lid again.
[][]Remove the sample after required period of time.

Cleaning

[][]Rub the desiccator, sample platform (desiccator plate) and lid with a dry, clean cloth.
[][]Laboratory Attendant will collect the silica (desiccant) to activate (in the oven at about 105°C) and then replace it to the desiccator once in a week or even more frequently when blue color of desiccant turns purple/pink.
[][]Fill up the logbook for desiccant change (as per Annexure-I).
[][]Officer/Executive, QC will check the logbook for proper condition of desiccant or the desiccant change.

Annexure:

Annexure-I: Logbook for desiccant change of desiccator.

Maintenance of Desiccator Read More »

Handling of Reference Standard and Preparation & Storage of WS

Quality Control, SOPs

Handling of Reference Standard; Purpose :

Handling of Reference Standard; The purpose of this procedure is to provide the instruction for handling of reference standard, impurity standards and standardization & storage of working standard.

Scope :

This procedure is applicable for the management of reference standard and working standard in the quality control laboratory of general block of XX Pharmaceuticals Ltd.

Definitions/Abbreviation:

Chemical Reference Standard:

Primary chemical reference standard is one that is widely acknowledged to have the appropriate qualities within a specified context, and whose value is accepted without requiring comparison to another chemical standard.

Secondary Reference Standard/Working Standard:

A secondary chemical reference standard is a substance whose characteristics are assigned and/or calibrated by comparison with a primary chemical reference standard. The extent of characterization and testing of a secondary chemical reference standard may be less than for a primary chemical reference standard.

[] CRS : Chemical Reference Standard
[] WS : Working Standard
[] USPRS : United States Pharmacopeia Reference Standard
[] BPCRS : British Pharmacopeia Chemical Reference standard
[] ICRS : International Chemical Reference Standard (WHO)
[] EPCRS: European Pharmacopeia Chemical Reference Standard

Responsibilities:

Officer/Executive, Quality Control

[] Handle reference standard properly according to manufacturer’s certificate of analysis and instruction.
[] To standardize working standard
[] ollow the instructions of this procedure correctly.

Sr. Executive, QC

[] To ensure proper handling & storage of reference standard andworking standard.
[] To keep a track of its use, use before date, current pharmacopoeias reference standard lot number and all the related documents.

Manager, Quality Control

[] To approve WS after verification.
[] To ensure appropriate personnel from the section are trained on this procedure.
[] To confirm that SOP is technically sound and reflects the required working practices.

Head of Quality Assurance

[] To ensure the overall implementation of the SOP.
[] Approval of the SOP.

Procedure:

General Note:

[] Read carefully the label of container before use of CRS.
[] After use sealed properly the CRS.
[] Handle the CRS according to material safety data sheet.
[] Ensure proper storage of CRS and WS.
[] Do not use CRS and WS after expiry.

Handling of Reference Standard:

Use one of the following Reference Standard for analysis of raw materials:
[] Pharmacopoeia Standards
[] Validated Suppliers Standards
[] In-house Reference Standards
[] Ensure that the purity of CRS is equivalent to 99.5% or higher, calculated on the basis of the material in its anhydrous form or free of volatile substances.
[] After receiving of CRS, write down the details in Chemical Reference Standard Details Record (as per Annexure-I).

[]During receiving, check the following points :

[][] Sealing condition (flip off seal for USPRS)
[][] Label on the container
[][] Part No.
[][] Lot No.
[][] Certificate of Analysis with complete information on test method.
[][] Information on optimal storage condition (Temperature and humidity).
[][] Updated material safety data sheet outlining any health hazard associated with the material.

[]Match the lot number of CRS with supplied vial.
[]Preserve all reference standard at 2-80C or according to the label of the container or according to manufacturer’s instruction.
[]Preserve all CRS up to expiry date.

[]Standardization of Working standard:

Determination of Identification:

[][]Use CRS for material identification by IR spectrometry and/or chromatographic methods.
[][]For identification, select a lot of respective raw material, which has been approved recently.
[][]Follow the approved analytical method for identification.
[][]Analyze the physical and chemical test against the reference standard.
[][]Confirm that the result is within specification and prepare the test report in Working Standard Analysis Report (as per Annexure-II).
[][]Use this lot as WS for the next routine analysis.

[]Determination of Assay:

[][]For standardization of WS, select a lot of respective raw material, which has been approved recently.
[][]Standardize this lot against the reference standard.
[][]Perform Water (by KF)/Loss on drying (whichever applicable) in twice as per specification and validated analytical method. The average of two results shall be used to determine the assay value.
[][]If the assay is performed by HPLC inject a blank, five replicate injection of standard solution, one test solution & one end standard. If the assay is performed by UV-Spectrophotometer or Potentiometer, at least analysis two samples. Percent of RSD for peak areas or readings of individual analyses should not be more than 1.0%.
[][]The content should be declared to two digits after decimal point.
[][]Prepare the report in Working Standard Analysis Report as per Annexure-II.
[][]Keep all relevant certificates of analysis, IR spectrum, chromatogram and any data regarding identification, purity and assay.
[][]A history sheet of each Working standards shall be maintained in Working Standard Preparation & Consumption Record (as per Annexure –III).

[]Labeling & Storage of Working Standard:

[][]After analysis kept sample in properly sealed clean and dry amber coloured glass vials/bottles.
[][]Prepare four vials/bottles of each working standard containing about 5 g.
[][]Prepare six vials/bottles of each working standard containing about 4 g in case of moisture sensitive materials.
[][]Affix the label on the WS Vials/bottles as per Annexure IV.
[][]On the opening of the vials/bottles, mention the date of opening on label.
[][]In order to maintain the integrity of the working standard, the dispensed vials/bottles have to be kept at the conditions indicated on the vials/bottles label. If the storage condition is 2ºC to 8ºC, store the dispensed vials/bottles in refrigerator with controlled temperature monitoring system and if the storage condition is recommended as room temperature, store the vials/bottles in a desiccator

[]Validity/Shelf Life and Consumption of Working Standard:

[][]Before preparation of working standard ensures that the manufacturer’s shelf life of respective material is valid up to more than one year.
[][]Use the working standard within one year from the date of standardization.
[][]Use the working standard of moisture sensitive material within two months from the date of opening.
[][]Use the working standard of non moisture sensitive materials within three months from the date of opening.
[][]Before use, keep refrigerated vials in a desiccator to reach at room temperature. After use seal the vial/bottle properly and store as per recommended storage condition.

[]Reference numbering system of Working standard:

[][]Assign working standard reference number in following way:
[][]Put first two letters of working standard i.e. WS.
[][]Put a hyphen (-) after the abbreviation, then a serial number of four digits i.e. 0001, again put a slash and then two digits of month i.e. 01 for January.
[][]Again put a slash (/) and then last two digits of the year i.e. XX for year 20XX.
[][]For example, First working standard prepare on January 20XX will get the Lab. Control No. WS-0001/01/XX

Discard Procedure of CRS & WS:

[][]At the time of issuing a new vial/bottle, the old/used vial/bottle shall be destroyed in following manner:
[][]Empty the contents in waste beaker containing previously prepared 0.4% sodium hypochlorite solution. Shake the dispersion of sample in container with the help of a glass rod and leave it for at least 12 hours. Then neutralize the liquid (pH 6-9) by acid/alkali and dilute the liquid 10 to 20% by fresh water and drain out slowly into designated place and clean the drain with adequate water flushing.
[][]Deface the label of the vial/bottle.
[][]Discard the vial/bottle into the specific container as broken glassware. Record the destruction details in Chemical Reference Details Record (as per Annexure-I) for CRS, and Working Standard Preparation & Consumption Record for WS (as per Annexure-III).

Annexure:

Annexure-I: Chemical Reference Standard Details Record
Annexure-II: Working Standard Analysis Report
Annexure-III: Working Standard Preparation & Consumption Record
Annexure-IV: Label of Working Standard

Handling of Reference Standard and Preparation & Storage of WS Read More »

Calibration of Glassware with Handling & Washing

Quality Control, SOPs

Calibration of Glassware: Purpose

Calibration of Glassware; The purpose of this SOP is to ensure that all glass wares are properly handled, thoroughly cleaned and calibrated accurately before use.

Scope:

This procedure is applicable for glassware handling, washing and calibration used in the different analysis of quality control laboratory and microbiology laboratory of general block of XX Pharmaceuticals Ltd.

Definitions/Abbreviation:

[] ASTM: American Society for Testing and Materials
[] SOP   : Standard Operating Procedure

Responsibilities:

[] Officer/Executive/Sr. Executive, Quality Control
[] To ensure that this procedure is followed.
[] To maintain the records properly as per SOP.

Manager, Quality Control

[] To ensure that this procedure is kept up to date.
[] To confirm that the SOP is technically sound and reflects the required working practices.
[] To arrange training on the SOP to all concerned personnel and to ensure implementation of the SOP after training.
[] Schedule calibration of the instrument at the defined intervals.

Head of Quality Assurance

[] Approval of the SOP.
[] To ensure the overall implementation of the SOP.

Procedure:

Precaution(s):

[] Handle with care during cleaning of Glassware.
[] Before discard of glassware, observe the label on glassware and handle with care as the type of chemical.
[] Wear gloves, mask and protective clothing during glassware handling and cleaning.
[] Do not use laboratory glassware for drinking purpose.
[] Do not handle the hot glassware without heat resistant gloves.
[] Do not put the hot glassware on cold or wet surface or cold glassware on hot surface.
[] Avoid to heat glassware that is etched, cracked, chipped, nicked or scratched.
[] Do not heat directly thin glassware with flaming.
[] Never place the glassware from the freezer into warm water baths.

Handling Procedure:

[] Hold the beakers, bottles, flask the side and bottoms rather than by the tops.
[] Avoid over tighten the clumps.
[] Use always coated clumps to avoid breakage while the clumping glassware.
[] Cool the glassware slowly to prevent breakage.
[] Dispose the broken glass into specific waste bucket.
[] Keep all cleaned glassware at designated place.

Washing Procedure:

[] Transfer all used glassware to washing area.
[] Discard the solution from glassware into a designated container/place.
[] Rinse initially all glassware with sufficient potable water for removal the residual content of solution.
[] For pipette, pass sufficient potable water through the pipette by force at two or three times.
[] Wipe to remove the label with detergent powder or suitable solution.
[] Allow to soak the glassware with diluted detergent for 10-15 minutes to remove any contaminants.
[] Rinse the glassware with sufficient potable water until detergent is removed.
[] Finally rinse with purified water for two or three times for removal any contaminating substances that may be present in the potable water.
[] Discard the rinsing solution.
[] Place cleaned glassware into Glassware drying rack for removal of residual water from glassware.
[] Dry the glassware for QC analysis and sterilize the glassware at 200°C for 1 hour for use in Microbiological analysis.

Calibration Procedure:

Burette Calibration:

[] Take a burette and inspect to ensure smooth tap operation.
[] Observe the tip of the burette, ensure no cracks or chips.
[] Observe markings on burette which is legible.
[] Rinse the burette at several times with purified water.
[] Fill the glassware up to the mark.
[] Dispense into a pre-tarred 100 ml beaker.
[] Record final volume.
[] Record mass of water.
[] Repeat the same procedure for another two times.
[] Calculate the volume delivered from the equation below using recoded weight and density of water at the temperature of calibration.  Take Tabulated Density of water at the temperature of calibration from the Annexure-II.
Volume of Burette= Weight/Tabulated Density of water at the temperature of calibration
[] Record calculated volumes, determine mean and compare the volume with that read from the burette and then determine the error as per Annexure – I.

Limit of error of the calculated volume should be as per following table (as per ASTM E-287)
Nominal Volume, mL2550
Limit of error, mL0.030.03
Limit of error, %0.120.10

Calibration of Pipette:

[] Take purified water into a beaker.
[] Record the temperature of the water used.
[] Weigh and tare another 100 ml beaker.
[] Dispense water as per pipette volume into tarred beaker.
[] Record the weight of purified water.
[] Repeat the same procedure for another two times.
[] Calculate the volume delivered from the equation below using recoded weight and density of water at the temperature of calibration.  Take Tabulated Density of water at the temperature of calibration from the Annexure-II.
Volume of Pipette= Weight/Tabulated Density of water at the temperature of calibration
[] Record calculated volumes, determine mean and compare the volume with the nominal volume and then determine the error as per Annexure – I.

Limit of error of the calculated volume should be as per following table (as per ASTM E-969)-
Nominal Volume, mL1234510152025
Limit of error, mL0.0060.0060.010.010.010.020.030.030.03
Limit of error, %0.600.300.330.250.200.200.200.150.12

Calibration of Volumetric Flask:

[] Observe the volumetric flask, ensure no cracks or chips.
[] Observe markings on volumetric flask, ensure they are legible.
[] Rinse volumetric flask at several times with purified water.
[] Rinse with acetone and air dry.
[] Tare volumetric flask on balance.
[] Add purified water and fill to mark.
[] Record weight of water.
[] Record the temperature of the water used.
[] Repeat the same procedure  for another two times
[] Calculate the volume delivered from the equation below using recoded weight and density of water at the temperature of calibration.  Take Tabulated Density of water at the temperature of calibration from the Annexure-II.

[] [] Volume of Volumetric Flask= Weight/   Tabulated Density of water at the temperature of calibration

Record calculated volumes, determine mean and compare the volume with the nominal volume and then determine the error as per Annexure – I.

Limit of error of the calculated volume should be as per following table (as per ASTM E-288)
Nominal Volume, mL
510255010020025050010002000
Limit of error, mL0.020.020.030.050.080.100.120.150.300.50
Limit of error, %0.400.200.120.100.080.050.050.030.030.025

Download All Annexure

Annexure I : Glassware Calibration Record
Annexure II : Density of Water

Calibration of Glassware with Handling & Washing Read More »

Analysis and Release Procedure of Intermediate and Bulk Product

SOPs

Analysis and Release Procedure: Purpose

Analysis and Release Procedure, The purpose of this procedure is to establish an appropriate system for analysis of intermediate stage sample (i.e. powder, granules, core tablet) and semi-finished (bulk) products (i.e. coated tablet, filled capsule) from production department for ensuring the quality by subsequent testing as well as releasing intermediate stage sample for next processing stage and semi-finished (bulk) products for packaging.

Scope:

This procedure is applicable for intermediate and semi-finished (bulk) products manufactured in general block at XX Pharmaceuticals Limited.

Definitions / Abbreviation:

Standard Operating Procedure (SOP): Standard Operating Procedure.

[] QC: Quality Control.
[] COA: Certificate of Analysis
[] SAF: Sampling Advice Form
[] Mfg. Date: Manufacturing Date
[] Exp. Date: Expiry Date
[] XX: Current version of SOP
[] Bulk Product: Any product which has completed all processing stages up to, but not including, final packaging.
[] Batch (or Lot): A defined quantity of material or product processed in one process or series of processes so that it could be expected to be homogeneous.

Responsibilities:

Sr. Executive/Executive, QC

[] To ensure that the instructions of this procedure are correctly followed.
[] To maintain the records properly as per SOP

Executive, QA

[] To perform sampling.
[] To provide SAF and sample to QC for analysis.
[] To receive report from QC dept. after completion of analysis.

Manager, Quality Control

[] To ensure that this procedure is kept up to date.
[] To confirm that the SOP reflects the required working practices.
[] To arrange training on the SOP to all concerned personnel and to ensure implementation of the SOP after training.

Head of Quality Assurance

[] Approval of the SOP.
[] To ensure the overall implementation of the SOP.

Procedure:

General Precaution(s):

[] Check the calibration status of the instruments to be used.
[] Check the validity of the working standard to be used.
[] Do not return any bulk sample to production unit to avoid batch/product mix-up.
[] Transfer excess sample to ‘Sample for Disposal’ place after approval.

Intermediate and Semi-Finished (bulk) Product Test Plan:

[] Before starting analysis ensure the test plan as Annexure-II.
[] In case of ready to fill pellets for capsule, carry out potency calculation by using assay result of representative lot of raw material & average filled weight (taken from in-process result of encapsulation stage). Dissolution test result will be taken from representative lot of raw material.
[] Perform assay & dissolution test in every 10th batch of regular commercial batch and process validation batch in case of ready to fill pellets for capsule.

Receiving and analysis:

[] Executive, Quality Assurance will collect sample of intermediate and semi-finished (bulk) product maintaining the SOP of intermediate and semi-finished (bulk) products sampling procedure.
[] Quality Assurance will provide test sample to QC according to ‘Intermediate and Semi-Finished (bulk) Product Test Plan’ (as per Annexure-II).
[] Executive, Quality Assurance will send test sample along with the Sampling Advice Form (SAF).
[] After receiving the sample, QC Executive will put the Lab. Control No. on the SAF and record all necessary information in ‘Intermediate and Semi-Finished (bulk) Product Log Register’ (as per Annexure-I).
[] After proper entry in the log book, QC Executive will keep the sample in the designated place of ‘Sample Receiving Room’.
[] QC In-charge/Sr. Executive, QC will assign the work and issue the finished product analytical work sheet to QC Sr. Executive/Executive with initial and date on every page and enter the worksheet issued by (initial and date) in the ‘Intermediate and Semi-Finished (bulk) Product Log Register’ (as per Annexure-I).
[] Sr. Executive/Executive, QC will take sample from sample receiving room and test the sample against the respective approved method of analysis.
[] Sr. Executive/Executive, QC will follow ‘Intermediate and Semi-Finished (bulk) Product Test Plan’ (as per Annexure-II) or as per requirement of SAF for analysis.
[] Record all analytical raw data and make calculation in the analyst logbook (Annexure-V) with attachment of required printout of weight(s).
[] Record the results in the work sheet with attachment of required raw data.
[] Carry out the test for assay of single sample preparation.
[] In case of instrumental analysis carried for testing, fill the instrument log properly.
[] Compare the results with the specification.
[] In case where test results go out of specification, report to designated personnel. Analysis may be repeated with proper authorization.

Release:

[] Sr. Executive/Executive, QC will compile the test report and prepare COA (as per Annexure-IV).
[] Sr. Executive/Executive, QC will check the test report, analyst log book, worksheet and COA.
[] In-charge, QC will verify the test report and approve COA if all results comply with the respective specifications.
[] If the test result does not comply with the specification follow the SOP for handling of out of specification.
[] After completion of the test, transfer left over sample in specified place labeled as “Under Test Samples” until the batch is approved.
[] After approval of the batch, transfer the excess sample to a place labeled as “Sample for Disposal” by making necessary entry in sample disposal register.
[] Sr. Executive/Executive, QC will input the necessary data in finished product trend analysis.
[] Send the approved test report with SAF and COA to Quality Assurance.

Find All Annexure Here

Annexure-I     : Intermediate and Semi-Finished (bulk) Product Log Register
Annexure-II    : Intermediate and Semi-Finished (bulk) Product Test Plan
Annexure-III   : Finished Product Analytical Worksheet
Annexure-IV   : Certificate of Analysis
Annexure-V    : Analyst Logbook

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Packaging Material Sampling and Release Procedure

Quality Control, SOPs

Packaging Material Sampling and Release, Purpose :

The purpose of this SOP is to describe the procedure for sampling and releasing of packaging materials for pharmaceutical products.

Packaging Material Sampling and Release, Scope :

This procedure is applicable for all packaging materials received at the warehouse of  XX Pharmaceuticals Limited.

Definitions/Abbreviation:

[] SOP: Standard Operating Procedure
[] QC: Quality Control
[] GRN: Goods Received Note
[] COA: Certificate of Analysis
[] ERP: Enterprise Resource Planning
[] Sampling: It is a process of collecting the materials so that the collection shall represent the whole lot.
[] Sampling plan: Description of the number of units and/or quantity of material that should be collected.
[] Consignment: A supply of a material of particular batch intended to be used in different department.
[] Lot: A defined quantity of material made by a specified process cycle having uniform quality.

Responsibilities:

The roles and responsibility is as follows:

Officer/Executive/ Sr. Executive, Quality Control

[] To ensure that the procedure is correctly followed.
[] To maintain the records properly as per SOP.
[] To ensure that this procedure is kept up to date.
[] To confirm that the SOP reflects the required working practices.
[] To arrange training on the SOP to all concerned personnel and to ensure implementation of the SOP after training.

Executive/ Sr. Executive, Warehouse

[] To ensure availability of containers to be sampled in quarantine area.

Executive, Production

[] To arrange machine trial when required and share the report to QC with the concern of Manager,

Production.

Head of Quality Assurance

[] To ensure the overall implementation of the SOP.
[] Approval of the SOP.

 Procedure:
General Precaution(s):

[] Take sample for microbial testing first followed by other sampling.
[] Sampling should be carried out by trained personnel.

Sampling: Packaging Material Sampling and Release

[] Receive the GRN with Manufacture’s COA from the warehouse and enter the details (GRN no., lab. control no., name of material, code no., invoice/challan no., manufacturer lot no., local batch no., manufactured by, supplied by, pack size, no. of pack, total quantity and received by & date) in the ‘Packaging Material Log Register’ (as per Annexure-I) maintained in QC department for packaging material.
[] Ensure that material is received from Approved Vendor.
[] If the material is not from approved vendor or if the Manufacture’s COA for primary packaging material is not received, inform Supply Chain Management Department.
[] QC Officer/Executive or QC sampler will select the no. of container/packs to be sampled as per sampling plan and sample quantity according to ‘Sampling quantity for Packaging Material’ (as per Annexure-II) and take required no. of “SAMPLED” label.
[] For example, when the total no. of container of inner carton (secondary packaging material) is 25, then no. of container to be sampled will be Ö 25 + 1 = 5 + 1 = 6.
[] If the batch size is 3100 pcs, then 32 pcs of inner cartons will be taken from 6 different containers.

Sampling plan:

[] The n plan

The “n plan” is based on the formula n = 1 + ÖN, where N is the number of sampling units in the consignment. The value of n is obtained by simple rounding. A minimum number of containers needs to be sampled, e.g. if N is less than or equal to 4, then every container is sampled. According to this plan, samples are taken from n sampling units (containers/pack) selected at random.

Sampling plan for primary packaging material

[] In case of primary packaging material, select no. of reels/pack/ container for sampling as per “n plan”.

Collect approximately 1 feet sample of foil/film from each of selected reels of films/foils.

[] In case of bottle/cap/dropper/stopper, take randomly 10 samples from selected containers.
[] In case of Container/Jerry can/Cap for Jerry can; check physical appearance of at least 3 samples from each selected container/pack (selected as per “n plan”) and then take randomly two containers for laboratory test from selected container/pack.

Sampling plan for secondary packaging material

[] For secondary packaging material, select container/pack for sampling as per “n plan”.
[] Samples can be withdrawn from any part of the container (usually from the top layer).
[] Collect sample proportionally from the selected container/pack following ‘Sampling quantity for Packaging Material’ (as per Annexure-II).
[] In case of Shipper carton and Master carton, check physical appearance and text of at least 3 shipper cartons from each selected pack and then take randomly 3 shipper cartons for laboratory test from selected pack.
[] Inform Warehouse before going for sampling to arrange the packaging material containers.
[] Take ‘Sampled’ label, sampling tools, packaging material sampling report, sampling basket and GRN before sampling.
[] Check the physical condition and cleanliness of packaging material containers/packs before opening for sampling.
[] If any container/pack found in damaged condition, intimate warehouse in-charge.
[] Damaged containers/packs whose integrity is doubtful should be sampled and tested separately.
Inform warehouse in-charge to take initiatives for repacking of damaged container/pack if necessary.

 Sampling of packaging materials

[] Check the details given on the GRN with the manufacturers label and ensure that the “Quarantine” label affixed properly by the warehouse personnel on all packaging material containers/packs of a consignment.

[] Check the physical condition of outer pack/container/damage condition.
[] Microbiology personnel will collect sample first in sampling booth for microbial analysis (when applicable).
[] Check the physical condition such as appearance (in case of Shipper carton/Master carton, Container/Jerry can/Cap for Jerry can), winding (in case of foil/film) etc. of the packaging material for any gross abnormalities. Measure internal core diameter, total reel diameter (in case of foil/film) of three reels. [] Record all necessary information in ‘Packaging Materials Sampling Report’ (as per Annexure-IV).
[] Select number of containers/bags/packs and collect sample according to sampling plan. Repair the sampling point properly, close the container/pack and affix the ‘SAMPLED’ label in cascading manner (overlapping upto half of the status bar of the previous label) over the “QUARANTINE” label without hiding any information of the previous label. Affix ‘UNDER TEST’ label on all other containers of the consignment in the same way.

[] Enter the information about the material sampled i.e. date, GRN No., lab. control no., name of  material, code no., invoice no./challan no., manufacturer lot no., manufactured by, sampled quantity, sampled by and remarks (if any)  into the ‘Sampling Register for Packaging Material’ (as per
Annexure-III).
[] Record sampling details in ‘Packaging Materials Sampling Report’ (as per Annexure-IV).
[] If any discrepancy found, immediately inform the warehouse in-charge to take action accordingly.
[] Transfer the collected samples to QC laboratory.

Release:

[] On receipt of the packaging material sample from warehouse, QC will keep them into “Under test sample (packaging material)” labeled rack in sample receiving room or any other designated place with proper labeling.
[] Enter the sampled by (initial) in the ‘Packaging Material Log Register’ (as per Annexure-I).
[] In-charge/Sr. Executive, QC will issue the packaging material work sheet with initial and date on every page to the analyst and enter the worksheet issued by (initial and date) in the ‘Packaging Material Log Register’ (as per Annexure-I).
[] Carry out the physical appearance test very carefully.
[] Test all parameters according to the packaging material specification and the packaging material test method and record the analytical raw data and calculations, and attach the printout of weight(s) in the analyst logbook.
[] Fill up the respective Packaging material work sheet (as per Annexure-V) and attach printout of required raw data.
[] Accordingly prepare the ‘Certificate of Analysis for Packaging Material’ (as per Annexure-VI).
[] Use bracket like [  ] to indicate that the result is taken from manufacturer’s certificate of analysis (COA).
[] Keep a remarks on ‘Certificate’, if any minor observation (variation in dimension, colour etc.) is found for a batch of packaging material.
[] Compile a batch report with COA, test report (packaging material work sheet), packaging materials sampling report (prepared as per Annexure-IV), QC copy of GRN.
[] Keep one retention sample with the bunch if feasible.
[] If it is not possible to keep retention sample with the bunch, keep them into another box/pack with proper labeling.
[] Submit the batch report with respective packaging material specification to Executive/Sr. Executive, Quality Control for checking.
[] Check and verify the test result against Packaging Material Specification. Inform production department for machine trial or practical trial for a particular material, if required.
[] Executive, Production is responsible for machine trial and reporting.
[] On completion of checking/verification, enter the detail in the ERP.
[] Submit GRN, testing report and COA to In-charge/Sr. Executive, QC for checking and approval. Give part release to fulfill the production demand, if required.
[] In-charge, QC/Sr. Executive, QC will check report and approve finally for passed/rejected status of the packaging material.
[] Officer/Executive, QC will prepare status label (Passed/Rejected) after approval of GRN. The expiry and retest should be not applicable for all secondary packaging materials, glass bottle, ampoule, plastic container/cap/dropper/stopper/syringe, polyethylene bag, aluminium cap, sealing foil and alu-lid foil. In case of PVC, PVdC film and Alu-bottom foil; the expiry and/retest should be as per manufacturer’s recommendation. If not mentioned by manufacturer, then the expiry period for PVC, PVdC film and Alu-bottom foil should be five years.

[] Officer/Executive/Sr. Executive, QC will check and sign on the passed label.
[] Only the rejected label will be signed by In-charge/Sr. Executive, QC.
[] After release of consignment entry information regarding a passed/rejected GRN in “Packaging material log register” (as per Annexure-I).
[] After approval send copy of GRN to warehouse/Store.
[] QC Executive or QC sampler will affix status label (Passed/Rejected) in cascading manner (overlapping upto 3/4 th of the status bar of the previous label) over the “SAMPLED” or “UNDER TEST” label without hiding any information of the previous label.
[] Enclose mail or any other relevant document and approved GRN, with the respective batch document.
[] Keep a copy of GRN with batch document and file it up.

List of Annexes: Packaging Material Sampling and Release Procedure

[] Annexure-I     : Packaging Material Log Register
[] Annexure-II    : Sampling quantity for Packaging Material
[] Annexure-III   : Sampling Register for Packaging Material
[] Annexure-IV   : Packaging Materials Sampling Report
[] Annexure-V    : Packaging Material Work Sheet
[] Annexure-VI   : Certificate of Analysis for Packaging Material

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Storage Conditions of Raw Materials and Packaging Materials

Quality Control, SOPs

Storage Conditions of Raw Materials and Packaging Materials, Purpose:

The purpose of this procedure is to describe the instruction of storage conditions of raw materials and packaging materials.

Storage Conditions of Raw Materials and Packaging Materials, Scope:

This SOP is applicable for storage conditions of raw materials and packaging materials to Quarantine Area, Ambient Store, AC Store, Finished Goods Store, Capsule Shell Store and Central Warehouse of XX Pharmaceuticals Ltd.

Definitions/Abbreviation:

[] Ambient Store: Storage area with normal environment condition.
[] MSDS: Material Safety Data Sheet.

Responsibilities:

The roles and responsibility is as follows:

Executive, Warehouse

[] Maintain storage conditions of all raw and packaging materials as per Manufacturer’s instruction or according to specification.
[] Record the temperature and humidity of the material storage room.
[] Follow the instructions of this procedure correctly.

Executive, Quality Compliance

[] Verify the storage conditions of raw and packaging materials.

 General Manager, Plant

[] Ensure that all raw and packaging materials are stored properly.
[] Ensure appropriate personnel from the section are trained on this procedure and evaluate the effectiveness of training.
[] Confirm that SOP is technically sound and reflects the required working practices.

Head of Quality Assurance

[] Approval of SOP.
[] To ensure the overall implementation of the SOP.

Procedure:
Precaution(s):

[] Precautions must be taken to prevent unauthorized entry in the storage areas.
[] All stores must be secured with lock and key.

Storage Conditions:

Maintain Storage conditions as below:
[] Quarantine Area :Below 25°C
[] Ambient Store:Below 40°C
[] AC Store:Below 25°C

Finished Goods Store:Below 30°C

Capsule Shell Store:Temperature Below 25°C & Relative Humidity Below 60%
Central Warehouse:Below 25°C

 Storage of the materials:

[] Carry out the emergency plan if temperature goes above 25°C for AC store.
[] Record the temperature and humidity for the time when temperature goes above 25°C.
[] Inform QA department immediately providing all recorded data and existing product status.
[] Check the recorded data and evaluate the sensitive material, which might temperature sensitive.
[] Send the advice to Quality Control Department for retesting of that sensitive material before use in production.
[] Carry out tests as described in the respective test method.
[] Analyze the impurity of the substance, if required.
[] Affix “REJECTED” label on the existing label of the container when retesting result does not comply with specification.
[] Prepare a list for storage condition of raw materials and packaging materials as per Annexure-VII; then take approval from Head of Quality Assurance.

[] Update the list for storage condition of raw materials and packaging materials three months to yearly or when required.

Recording of storage conditions:

[] Sr. Executive/Executive, Quality Compliance will issue the ‘Temperature & Relative Humidity Record Sheet of Warehouse’ as per Annexure-I to Annexure-VI
[] Executive, Warehouse by maintaining proper record.
[] Record the temperature and humidity of Quarantine Area, Ambient Store, AC Store, Finished Goods Store, Capsule Shell Store and Central Warehouse thrice in a day in ‘Temperature & Relative Humidity Record Sheet of Warehouse’ prepared as per Annexure-I to Annexure-VI.
[] Maintain the storage condition as per QA approved Storage Condition of Raw materials and Packaging materials.

List of Annexes

1.0 Annexure-I: Temperature Record Sheet of Quarantine Area.
2.0 Annexure-II: Temperature Record Sheet of Ambient Store.
3.0 Annexure-III: Temperature Record Sheet of AC Store.
4.0 Annexure-IV: Temperature Record Sheet of Finished Goods Store.
5.0 Annexure-V: Temperature & Relative Humidity Record Sheet of Capsule Shell Store.
6.0 Annexure-VI: Temperature Record Sheet of Warehouse Central Warehouse.
7.0 Annexure-VII: Format of Storage Condition of Raw materials and Packaging materials.

 

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