Sop for Calibration of Dissolution Apparatus
It describes the (Standard Operating procedure) Sop for Calibration of Dissolution Apparatus
Sop for Calibration of Dissolution Apparatus
I. Purpose & Scope:
- The purpose of this document is to lay down the procedure of Calibration of Dissolution Apparatus.
- This procedure is applicable for Calibration of Dissolution Apparatus used in Quality Control Department.
II. Responsibilities:
- All Quality control personnel shall be responsible to follow and implement this SOP i.e. Calibration of Dissolution Apparatus
III. Introduction and Procedural part:
General Cleaning before performing Calibration of Dissolution Apparatus :
- Clean the instrument with a clean dry cloth every day. Occasionally wet cloth dipped in dilute soap solution furthermore wet cloth dipped in purified water may be used.
- A precaution has to be taken to clean the instrument immediately with dry cloth to remove the moisture.
Basic Operation while Calibration of Dissolution Apparatus :
- Ensure that the instrument is properly connected to the power supply.
- Ensure that the tank is filled with purified water up to the mark of the instrument.
- Switch ON the machine.
- Lift the stirrer unit using the lift switch. Fill the vessels with the appropriate medium as mentioned in the Standard Testing Procedure.
- Fix the paddles or basket stirrers on the spindle carefully and tighten them.
- Set up program ‘01’ as per the Standard Testing Procedure.
- Press the ‘temp key’ & set up the temperature as per the requirement and then press ‘start temp’.
- Press the ‘timer key’ and set up the time as per the requirements and then press ‘start timer’.
- Press ‘RPM key’ and set up the RPM as per the requirement and then press ‘start RPM’.
- After the instrument set up wait till the instrument shows ‘Ready’ on display’.
- Stop the RPM and place one tablet/capsule in each of the basket stirrer at up lift position and bring the stirrer unit down using the lift switch. In case of paddle stirrer place the tablet/capsule in the Dissolution jar after bringing the stirrer unit down and start immediately the stirring after covering the vessels with lids. Sinker shall be used if dosage unit floats or as required
- At the given time interval specified in the individual STP withdraw a sample from a dissolution medium at below center of basket or paddles.
- Filter samples through Whatman No.1 filter paper and follow the individual Standard Testing Procedure.
- Clean all the vessels and stirrers after completion of the analysis and switch OFF the instrument.
- Maintain the instrument usage log book as per SOP Handling of instrument usage log book.
Calibration of Dissolution Apparatus :
Calibration Frequency for Dissolution Apparatus :
Physical Parameter:
Once in six months and after each maintenance job.
Apparatus suitability test:
Once in Year with USP dissolution calibrator i.e. Prednisone tablets USPRS.
Physical Parameter :
- RPM: Paddle and basket measuring revolutions per minute (with a standard clock) at two different RPMs.
- Acceptance Criteria for RPM : ±2 % of set RPM (Set RPM 50 to 100)
- Temperature: It shall be validated by standard, calibrated thermometer.
- Acceptance Criteria for Temperature : ± 0.5°C of set temp. (Set temp. 37°C)
- Timer: Instruments timing can be checked with standard stop watch.
- Paddle/Basket to Jar bottom height: Use the Calibrated vernier caliper with special attachment.
- Acceptance Criteria for Jar bottom Height : 25 ± 2 mm
- Wobble & Centering: Both the parameters can be simultaneously checked by the dish tool.(By Wobble Meter).
- Acceptance Criteria for Wobble and centering : Not more than 2 mm
- Coplanarity: It compromises level and perpendicularity.
- Level: Assure the platform level first the instrument level.(Take two different readings at 90° to each other).
- Perpendicular: Check the perpendicularity (Paddle and basket shaft must be perpendicular to the base plate and head plate)of the paddles by using a T square. (Take two readings at 90° to each other).
- Record the Observation in Calibration Record in Annexure I & II.
Apparatus Suitability test :
- Performance verification test using dissolution calibrator disintegration type prednisone tablets USP 10 mg.
- Use current lot of USP dissolution calibrator disintegrating type Prednisone tablets 10 mg.
- Store in original container as per the recommended storage condition. Do not expose the tablets in excessive humid conditions.
- Cracked, chipped, capped tablets should not be used for calibration.
- Powder on the surface of tablets should be removed by soft brush prior to use.
- Either Set the dissolution parameter as per the method specified in the documents received along with the respective lot of tablet or the apparatus shall be operated at a temperature 37°C ± 0.5°C, 50 RPM for 30 minutes.
- Dissolution Medium : Deaerated purified water 500 ml.
- Deaeration of dissolution medium: Heat a suitable amount of medium, while stirring gently, to about 45°C, filter under vacuum using a filter having a porosity of 0.45µm or less, with vigorous stirring, and continue stirring under the vacuum for about 5 minutes. Do not allow the temperature of the dissolution medium to fall below 37°C prior to initiation of the test. Gently transfer the medium directly to the vessel.
- Reference Standard Preparation : Accurately weigh and transfer about 10mg of Prednisone reference standard in to a 100 ml volumetric flask, add 5ml of ethanol to dissolve, dilute up to the mark with purified water. Dilute 10 ml of this solution to 50 ml with purified water.
- Conduct the performance verification test at condition mentioned in the certificates of tablets using Basket (USP type apparatus-I) and Paddle (USP type apparatus-II).
- After completion of the dissolution time withdraw the aliquot and filter with membrane filter.
- Discard the first 2 ml of solution and measure the absorbance the filtrate portion for concentration of Prednisone at 242 nm against the Prednisone reference standard solution.
- Record the observation in Annexure I
- Calculate the percentage amount of Prednisone dissolved by using following formula.
AT WS 10 500 P
——- X ———X ———-X ———–X ———X100
AS 100 50 1 10
- The % release shall be determine for each tablet (6 Tablets)
- Calculate the GeoMean (Upper and Lower) and % CV (Upper) from % release observed for Prednisone tablets of used USP RS lot. Follow the procedure as below
- Go to browser and type usp.org and enter.
- USP main window will open. Select country as USP India.
- Move the mouse cursor to “Our Work” icon and click on “Chemical Medicines”
- On left side of window “Performance verification Test” icon shall be displayed; click this icon.
- In next window; select the “PVT calculation tool” then click on “Access Tool”. New window shall be open of U.S. Pharmacopoeial convention form calculation tool for performance verification test calculations.
- Tick on terms of use and click on submit icon.
- Select the lot used for test in dropdown box.
- Select the apparatus Basket or Paddle using for calculation.
- Select the configuration of dissolution test assembly using. E.g. 6 or 12.
- Choose the testing procedure you will be using to perform your calculation e.g. 1-Stage.
- Click on “Submit Data”, next window will open.
- Enter the details of date performed, operator, Assemble ID, Note book (Company name) and notes (Optional – not mandatory).
- Enter the % release of drug determined by using above formula mentioned of 6 vessels. Then click on “Submit Data”; new window will open.
- The test results shall be displayed on screen.
- The combined Geo Mean and combined % CV value shall be displayed on screen. The value shall be meets with the acceptance criteria for USP Prednisone Tablets of used lot.
- Click on printable version and take the print out and enter the details in Annexure I.
- If Acceptance criteria does not meets the criteria then perform the stage 2 analysis by using Prednisone tablets.
- If the calibration of instrument is within the predefined acceptance criteria then affix a calibration status label.
- When the instrument does not comply with the requirement/acceptance criteria, the instrument shall be labeled as out of calibration and immediately inform to Manager Quality control.
- Handle the out of calibration results as per Specified SOP.
- Acceptance criteria: The apparatus is suitable if each of the individual calculated values for each apparatus at indicated speed is within the specified range.
IV: Annexure:
Annexure I : Calibration of Dissolution apparatus Record for Suitability Test.
Annexure II : Calibration of Dissolution apparatus for physical Parameter
Annexure -I
Calibration of Dissolution apparatus for Suitability Test
| Name of Instrument : Dissolution Test Apparatus | Make : |
| Instrument ID No : | Model : |
| Calibration done on: | Calibration Due on: |
- A) Cleanliness of the Instrument:
Observation: Clean / Not Clean
- Any other maintenance:
Observation: Required / Not required
- B) Performance verification test using dissolution calibrator disintegration type Prednisone tablets USP:
| Lot No. of Prednisone tablet USP: ______________________Valid up to: ______ | ||||||||||||
| Lot No. of Prednisone USPRS :________________________ Valid up to: _____ | ||||||||||||
| Balance ID No.: ______________________ Calibration Due On:____________
SOLUTION PREPARATION : Preparation of Standard Solution : Weight and transferred __________ mg (about 10 mg) of prednisone reference standard in to _______ ml (100 ml) volumetric flask, ________ ml (5 ml) of ethanol to dissolve and diluted up to mark with purified water. Further diluted _______ml (10 ml) of this solution 50 ml with purified water. Preparation of Test Solution (For Paddle USP type II) : Placed _______ (1) tablet in _________ ml (500 ml) of dissolution medium in each of six dissolution jars. After completion of the dissolution withdraw the aliquot and filtered with completion of the dissolution with 0.45 µm membrane filter.
Dissolution Parameter :
|
Calculation Formula:
Spl. Absorbance Std.Wt( mg) 10 500 Std Purity(%) 100
% Release = ———————– x ——————-x——–x——- x —————— x ——————–
Std Absorbance 100 50 1 100 Label Claim(mg)
| Standard/Test Unit | Absorbance | % Release |
| Standard | ||
| Test Unit-1 | ||
| Test Unit-2 | ||
| Test Unit-3 | ||
| Test Unit-4 | ||
| Test Unit-5 | ||
| Test Unit-6 |
Remark: Performance verification of dissolution test apparatus using Prednisone tablets USP by apparatus-II (paddle) is Complies / does not comply.
CALIBRATED BY (QC ): CHECKED BY (Head QC): CHECKED BY (Head QA):
DATE : DATE : DATE :
Preparation of Test Solution (For Basket USP type I):
Placed _______ (1) tablet in ________ ml (500 ml) of dissolution medium in each of six dissolution jars. After completion of the dissolution withdraw the aliquot and filtered with completion of the dissolution with 0.45 µm membrane filter.
Dissolution Parameter:
| Dissolution Medium : | |
| Volume : | |
| Apparatus : | |
| Speed : | |
| Time : | |
| Temperature : |
Calculation Formula:
Spl. Absorbance Std. Wt ( mg) 10 500 Std Purity(%) 100
% Release = ———————– x ——————-x——–x——- x —————— x ——————–
Std Absorbance 100 50 1 100 Label Claim(mg)
| Standard/Test Unit | Absorbance | % Release |
| Standard | ||
| Test Unit-1 | ||
| Test Unit-2 | ||
| Test Unit-3 | ||
| Test Unit-4 | ||
| Test Unit-5 | ||
| Test Unit-6 |
Remark: Performance verification of dissolution test apparatus using Prednisone tablets USP by apparatus-I (Basket) Complies / does not comply.
Conclusion: The instrument is calibrated as per SOP and Complies / does not comply with the acceptance criteria
Calibrated By: Checked By: Approved By:
Date: Date : Date :
Annexure-II
Calibration of Dissolution apparatus for Physical Parameter
| Name of Instrument : Dissolution Test Apparatus
|
Make : |
| Instrument ID No : | Model : |
| Calibration done on: | Calibration Due on: |
A) Cleanliness of the Instrument:
Observation: Clean / Not Clean
- Any other maintenance:
Observation: Required / Not required
- Adjustment of Water level:
Observation: Done / Not done
CALIBRATED BY: CHECKED BY:
DATE : DATE :
B) Physical Observation :
| Bath Horizontal Level | Perpendicularity level | Test
Unit |
Paddle
Wobble (Not more than 2 mm) |
Paddle
Centering (Not more than 2 mm) |
Paddle to jar bottom Height
(25 ± 2 mm) |
Basket to jar bottom Height
(25 ± 2 mm) |
| 1 | ||||||
| 2 | ||||||
| 3 | ||||||
| 4 | ||||||
| 5 | ||||||
| 6 |
Remark: Complies / Does not comply
CALIBRATED BY: CHECKED BY:
DATE : DATE :
C) PHYSICAL VERIFICATION:
| Timer | Paddle Rotation | Temperature
37 ± 0.5°C |
|||
| Set Time | Observed Time | Test
Unit |
50 ± 2 rpm | 100 ± 2 rpm | |
| 1 | |||||
| 2 | |||||
| 3 | |||||
| 4 | |||||
| 5 | |||||
| 6 | |||||
Remark: Complies / Does not comply.
Conclusion: The instrument is calibrated as per SOP and Complies / does not comply with the acceptance criteria.
Calibrated By: Checked By: Approved By:
Date: Date: Date:
Note : Calibration of Dissolution apparatus shall be done as per Standard operating procedure
