Calibration of Dissolution Tester Purpose :
Calibration of Dissolution Tester; The purpose of this SOP is to describe the operation, calibration and cleaning of Dissolution Tester (Model: Electrolab, TDT-08L).
Scope :
This procedure is applicable for Dissolution Tester (Model: Electrolab, TDT-08L), installed in the quality control laboratory at general block of XX Pharmaceuticals Limited.
Definitions/Abbreviation:
[][]SOP: Standard Operating Procedure
[][]QC: Quality Control
[][]Dissolution test: Dissolution test is a means to monitor the rate of release of a drug substance from a dosage form to ensure consistency of manufacture and compliance with release specifications.
[][]RPM: Rotations per minute
[][]LED: Light emitting diode
[][]Concentricity: The quality of having the same center (as circles inside one another)
[][]Wobble: Move sideways or in an unsteady way
[][]NMT: Not more than
Responsibilities:
The roles and responsibility is as follows:
Officer/Executive/Sr. Executive, Quality Control
[][]To ensure that the instructions of this procedure are correctly followed.
[][]To ensure cleaning of dissolution tester maintaining safety rules.
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:
[][]General precautions or operational safety:
[][]Do not start the heater if there is no water in the tank.
[][]Always maintain the liquid level within the tank above the minimum level mark using purified water only.
[][]Disconnect the power supply before moving, emptying or cleaning of bath.
[][]Spillage must be cleaned up immediately after use.
[][]Do not use any aggressive material or strong solvent to clean the jar and water bath.
[][]Locate the system on a level bench without movement or distortion.
[][]Do not hold the stirrer while in operation.
[][]For lifting up the stirrer, make sure the paddles are stop.
[][]Do not disturb the sensor tube while cleaning the tank.
[][]External probe should be handled with care.
[][]Use sinkers if the dosage form unit floats. Close the vessels with the cover during Operation.
Operation:
[][]Connect the instrument to the main power supply.
[][]Ensure the calibration status is valid.
[][]Lift the head by approximately 20 cm by pressing lift UP arrow push button.
[][]Fill the purified water in the tank up to the mark level without jars. Place the tank on the base of the instrument such that four screws at the bottom of the tank fits in to the holes on the base plate and heater cable is at the rear side of the instrument.
[][]Connect the heater plug in the socket provided at the right hand side of the stirrer unit. Add 0.01% Cetyl puridinium chloride or Sodium benzoate or Bronidiol to prevent fungal growth in the water bath.
[][]Connect the power cord from the ETC-11L to TDT-08L in the socket provided on the rear side of the instrument.
[][]Turn on the red colored power switch provided on the front side of ETC-11L.
[][]The yellow colored switch of the Heater will remain always on.
[][]Switch on the power switch provided on the rear
ELECTROLAB
TDT-08L VER 3.50C
DISSOLUTION
TEST APPARATUS
[][]After the power flash screen an idle screen will be displayed showing the last Mode. Protocol no. selected, RPM, Bath temperature and Temp by external probe.
[][]There are 20 protocols. We can assign 20 types of samples against these protocols.
[][]Set the protocol with // keys.
[][]Insert the test vessels in the water bath.
[][]Insert the paddles/basket in the stirrer unit.
[][]Press TEMP key from the front panel. Temperature setting screen will be displayed.
[][]Using // key set the temperature. Set the temperature to 37.7ºC so that the jar temperature reaches to 37ºC.
[][]Press F1 to on the heater. The [Temp. ON] indicator will flash on.
[][]Press ENTER key to register the temperature and come out of the TEMP mode. An idle screen will be displayed.
[][]Press RPM key. Adjust the RPM with // keys.
[][]Press ENTER to register the RPM and come out of the screen.
[][]To set the time press TIME key. A screen will appear like
SAMP. No = 00 OF 00
SAMP. INTV. = 00 Hr: 00 Mn
[][]Set the sampling number 01 OF 01. Set total dissolution time (as per test method for a particular product) in SAMP. INTV by using // keys.
[][]Press ENTER key to register the time and come out to the initial screen.
[][]Wait to raise the bath temperature up to the desired level.
[][]When the temperature will raise to desired level the [READY] indicator will flash on.
[][]Add dissolution media into individual test vessel as per test method. Measure media temperature with the sensor. Wait until the temperature reaches to 37 ± 0.5°C.
[][]Place sample in vessels in case of paddle apparatus taking care to exclude air bubbles from the surface of the dosage form unit.
[][]In case of basket apparatus place sample in dry baskets, attach the shaft into stirrer unit and lower down the stirrer unit into medium. By lift DOWN key.
[][]Immediately press START key to run the operation.
[][]The screen will show the Elapse time of operation.
[][]After completion of the time interval the instrument will give beep sound.
[][]Lift the stirrer using the lift UP key.
[][]Withdraw the dissolution medium with suitable pipette from a zone midway between the surface of the dissolution medium and the top of rotating paddle through the head nozzle, not less than 1 cm from the vessel wall.
[][]The sampling has to be filtered immediately after completion of the sampling.
[][]After completion of work, switch ‘OFF’ the instrument.
[][]Switch ‘OFF’ the mains when not required.
[][]Fill up the operation log book for Dissolution tester as per Annexure-III.
Physical Calibration
Frequency: Perform mechanical calibration of the dissolution tester once in every six months or if the system has been moved, serviced or a malfunction is suspected.
For Temperature Calibration:
[][]Switch on the mains
[][]Set the temperature to 37°C by following the temperature setting procedure given in operation.
[][]Ensure that the jars are filled with water
[][]Allow the instrument to stabilize
[][]Measure the temperature of the water bath and of each jar with a calibrated thermometer and compare the result against the digital display on the apparatus.
[][]Record the observation as per Annexure-I.
[][]Acceptance Criteria: 37°C ± 0.5°C.
For RPM Calibration:
[][]Switch on the mains.
[][]Set the RPM to 50 as per procedure given in the operation.
[][]Start the stirrer and measure the RPM by using calibrated tachometer.
[][]Record the observation as per Annexure-I.
[][]Similarly check the RPM 75, 100, and 150 and record the observations.
[][]Acceptable criteria: ± 4% of set value.
For Time Calibration:
[][]Switch on the mains.
[][]Set the desired time (30 and 45 Minutes) by following the temperature setting procedure given in operation.
[][]Check the time using a calibrated stop watch and record the observations as per Annexure-I.
[][]Acceptable criteria: ± 2% of set value.
Chemical Calibration (Dissolution Performance Verification Testing)
Frequency: Perform chemical calibration of the dissolution tester once in a year or if the system has been moved, serviced or a malfunction is suspected.
For USP Dissolution Apparatus 1 (basket) and Apparatus 2 (paddle):
[][]If the instrument is outside calibration, a label of “Out of calibration” is placed.
[][]Apparatus must be calibrated with the following :
Disintegrating Type – USP Prednisone Tablets 10 mg at 50 rpm
[][]Non-disintegrating Type – USP Salicylic Acid Tablets 300 mg at 100 rpm
[][]Checking Standards in the on line-USP and printing Lot-Specific Standard Certificates. Verifies Standard Lots are current within expiry.
[][]Disintegrating Type – USP Prednisone tablets 10 mg at 50 rpm:
[][]Follow the directions for storage and use on the label of the reference standard.
[][]If drying instructions are included on the label, only dry sufficient quantity required for the test (use a clean, dry vessel when drying and not the original container).
[][]Standard solutions must be prepared on the day of use.
Prednisone Standard Preparation (Standards must be prepared in duplicate):
[][]Accurately weigh 20 mg Prednisone standard into a 100 ml volumetric flask containing 5 ml of methanol.
[][]Sonicate to dissolve and dilute to volume with distilled or purified water and mix well.
[][]Further dilute 5.0 ml of this solution to 100 ml with distilled or purified water and mix well.
Dissolution Medium Preparation and De-aeration:
[][]Filter the dissolution medium (Distilled or purified water 500 ml) with the aid of a vacuum through a 0.45 µm-porosity membrane filter into a suitable filtering flask.
Test Procedure:
[][]Using a volumetric flask, measure 500 ml distilled or purified water into each of the six vessels.
[][]Allow medium to equilibrate for approximately 30 minutes before test is commenced.
[][]When dissolution bath has equilibrated, check the temperature of each vessel is 37.0°C ± 0.5°C.
[][]Carefully weigh 6 de-dusted USP Prednisone Tablets 10 mg.
[][]Drop one previously de-dusted tablet into each of the vessels via the sample holes in the lids, raising the stirrer shaft fully before dropping the tablet into the vessel, and pushing the shaft fully down when the tablet has reached the bottom.
[][]Operate the apparatus at 50 rpm for 30 minutes.
[][]After 30 minutes withdraw approximately 50 ml midway between the surface of the dissolution medium and the top of the blade, not less than 1cm from the vessel wall.
[][]Filter through a Whatman Number 1 filter paper, discarding the first few ml of filtrate.
[][]Scan the standard from 300-200 nm to obtain the maximum absorbance at the optimum wavelength (approximately 242 nm).
[][]Determine the absorbance of the six samples at that wavelength in fixed mode.
[][]Calculate the percentage prednisone dissolved for all 8 stations using the following calculations:
Absorbance of Sample x Standard Concentration (mg/l) x Standard Potency x 100] divided by
[Absorbance of Standard x Sample Concentration if 100% dissolved (C100) x 100]
Acceptance Criteria:
[][]Check the percentage released limit of USP dissolution calibration tablets (Disintegration type: Prednisone tablets) from the respective batch certificate provided by USP.
[][]If any one station is outside of specification, place an “Instrument out of calibration, DO NOT USE” label on the instrument.
[][]Inform In-charge, QC; if the results do not meet the criteria.
Test interpretation:
[][]The apparatus shall be suitable if the individual calculated values at each indicated speed are within the range specified in the tablet obtained with the each lot of tablets.
[][]Note: An amount of alcohol not to exceed 5% of the total volume of the standard solution may be used to bring the prednisone standard into solution prior to dilution with dissolution medium.
Recording of Results:
[][]All relevant information on the calibration must be completed on Annexure-II.
[][]When all the results have been checked affix a Calibration label to the instrument.
Cleaning procedure
[][]Lift the stirrer unit by using “lift UP” key.
[][]Switch ‘OFF’ the heater.
[][]Switch ‘OFF’ the instrument.
[][]Switch ‘OFF’ the mains.
[][]Remove the plug from the main socket.
[][]De-dust the outer surface of the instrument with a clean dry cloth every day.
[][]Clean apparatus after completion of every dissolution test.
[][]Remove the test vessels from their place and discard the medium.
[][]Wash each vessel with purified water and then set them inside the dissolution bath number wise.
[][]Remove basket/paddle apparatus from the dissolution tester. Wash them with purified water and dry with tissue paper and keep at dedicated place.
[][]Clean and replace the water from dissolution bath fortnightly (once in every two weeks) or if necessary.
[][]Remove all vessels from the dissolution bath.
[][]Remove the basket/ paddle apparatus from the stirrer unit.
[][]Remove the circulating pipe which is provided at the right rare side of the dissolution bath.
[][]Start the circulation pump from the option menu and drain the dirty water in a waste water bucket.
[][]Insert the circulating pump in its proper place.
[][]Wash the dissolution bath with potable water, detergent solution and then again with potable water sequentially until no foam of detergent remains in the bath.
[][]Wash the bath finally with purified water and fill the bath with the same up to the level mark.
Annexure Download Here
Annexure-I: Physical Calibration Information Sheet for Dissolution Teste
Annexure-II: Chemical Calibration Information Sheet for Dissolution Tester
Annexure-III: Operation Log book for Dissolution Tester