dissolution test system validation · pdf filei agree that the iq, the oq and the pq...

distek

©

DISSOLUTION TEST SYSTEMVALIDATION LOGBOOK

DISTEK Unit SN

Version 20020416 REV 4

mailto:[email protected]

http://www.riggtek.de

Francesco

SAMPLE COPY

Version 20020416 REV 4 Printing Date: 12 May 2005 of 35

DISTEK Dissolution Test System Validation Logbook Unit SN:

Deviations YES: NO: Verified by Customer:

CONTENTS

1 Document Authenticity ....................................................................................5

2 Protocol Approval ............................................................................................6

2.1 Protocol Acceptance of the Customer ................................................................... 6

2.2 Protocol Acceptance of the Qualification Engineer .............................................. 6

3 Document Control ........................................................................................7

4 Document Scope.............................................................................................8

5 Design Qualification (DQ)................................................................................9

5.1 System Purpose ....................................................................................................... 9

5.2 Instrument Features................................................................................................. 9

5.3 Operational Specification ........................................................................................ 9

5.4 Conformance Statement.......................................................................................... 9

5.5 System and Process Description............................................................................ 9

5.6 System Validation Conclusions.............................................................................. 9

5.7 Use of the Operational Qualification (OQ)............................................................ 10

5.8 Use of the Performance Qualification (PQ).......................................................... 10

5.9 Recommended periods of OQ and PQ and preventive maintenance ................ 10

6 Installation Qualification (IQ) .........................................................................11

6.1 Customer Details and Reconciliation against Purchase Order.......................... 11

6.2 Identity of the Unit, Firmware and individual Operation Manual ........................ 12

6.3 Qualifying of the Site ............................................................................................. 12

6.4 Qualifying of the Cable and Tubing Connections ............................................... 12




© DISTEK Dissolution Test Systems, Am Heidebruch 13 b, D-81375 München

6.5 Installation Procedures.......................................................................................... 12

6.6 Additional Comments ............................................................................................ 13

6.7 IQ Completion......................................................................................................... 13

7 Operational Qualification (OQ)......................................................................14

7.1 Level Check ............................................................................................................ 14

7.2 Shaft and Vessel ID ................................................................................................ 15

7.3 Height Check Baskets............................................................................................ 16

7.4 Height Check Paddles............................................................................................ 17

7.5 Center and Wobble Check..................................................................................... 18

7.6 RPM and Vibration Check...................................................................................... 20

7.7 Temperature Check................................................................................................ 22

7.8 System Control Check (Timing) ............................................................................ 24

7.9 Summary Sheet ...................................................................................................... 25

7.10 Calibration Equipment ........................................................................................... 25


7.12 OQ Completion....................................................................................................... 26

7.13 OQ Record .............................................................................................................. 27

7.14 Training Certificate Record ................................................................................... 28

8 Performance Qualification (PQ) ....................................................................29

8.1 USP Calibrator Tablet Test .................................................................................... 29


8.3 PQ Completion ....................................................................................................... 30

8.4 PQ Record............................................................................................................... 31




9 Maintenance Qualification (MQ)....................................................................32

10 Service Record...........................................................................................33

11 Operator Record.........................................................................................34

12 Training Policy............................................................................................35




1 Document Authenticity

The authenticity of this document is assured by:

(1) The Document ID is on each page of the DISTEK Dissolution Test System ValidationLogbook.

(2) The Instrument Serial Number, printed or written on the head of the page, identifies eachcopy of the DISTEK Dissolution Test System Validation Logbook and assigns it to a specificinstrument.

(3) RIGGTEK has signed (facsimile) in the chapter Document Control.

If a copy of the DISTEK Dissolution Test System Validation Logbook does not include all above-mentioned features, the copy should be regarded as a non-authentic document.

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mailto:[email protected]

http://www.RIGGTEK.de

Francesco

SAMPLE COPY




2 Protocol Approval

Use this Protocol Approval to qualify and record the Installation, the Operational Qualification and thePerformance Qualification of the DISTEK Dissolution Test System Unit.

2.1 Protocol Acceptance of the Customer

A signoff area is provided at the bottom of each page in case an internal SOP requires the review andthe acceptance of every page in this document. If page-by-page signoff is not required, use the area atthe bottom of each page to document deviations only.

The acceptance of the entire document is complete when the Certification of the System Qualificationis reviewed and the Protocol Approval is signed by the responsible parties.

Certification of the System Qualification:

Page-by-page signoff Yes/No

Required

Required only for pages that contain data

Required only for pages that contain deviations

I have reviewed this document and agree that it provides appropriate procedures for the IQ, the OQand the PQ of the equipment for which it has been configured.

Customer Name (Print) Signature Date

Additional review, if required by the customer.

Reviewer Name (Print) Signature Date

2.2 Protocol Acceptance of the Qualification Engineer

I agree that the IQ, the OQ and the PQ procedures in this document, assembled by DISTEK, Münchenand RIGGTEK, are appropriate for the equipment defined within and reflect the current DISTEK,München and RIGGTEK qualification procedure.

Qualification Engineer Name (Print) Signature Date




3 Document Control

Prepared By: RIGGTEKConsulting * Laboratory InstrumentsAm Heidebruch 13 bD-81375 München

Authorized By: Dipl.-Ing. Hansjürgen Riggenmann

Signature (facsimile):

Document: DISTEK Dissolution Test System Validation Logbook

Issue Number: 20020416

Originated: 16th April 2002

Amendment Record: Document Revision History

Document Revision History:

REV Date Notes

1 16th April 2002

2 27th October 2003 Dissolution Model Range increased

3 7th July 2004 Complete Validation Logbook corrected

4 5th October 2004 Protocol Approval section added

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4 Document Scope

This document is intended to provide a validated record of the DISTEK Dissolution Test SystemUnit throughout its operational lifetime via a structured framework designed to allow completedocumentation of the system.

The DISTEK Dissolution Test System Unit is available under the following Trade Names (andextensions), which are fully covered by this document:

§ DISTEK Premiere 5100 Dissolution System (“bathless”) and successors

§ DISTEK Dissolution Test System Model 2100 series (conventional bath) andsuccessors

The DISTEK Dissolution Test System Units can be operated as a stand-alone system or can beintegrated with an online or offline sampling and analysis setup. The scope of this ValidationLogbook is limited to providing Physical Qualification of the Unit as a stand-alone system onlywith no accessories interfaced.

It covers all aspects of the system from design criteria through installation, operation and maintenancewith emphasis placed on the role of the suppliers in assisting the customer to meet all equipmentqualification requirements.

Within this document ……DISTEK, München……………………………………… (Executing Engineer)and RIGGTEK (Owner of Production and Sales Rights) will provide all necessary defined protocolssuitable for implementing pre-planned calibration and maintenance programs.

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5 Design Qualification (DQ)

5.1 System Purpose

The DISTEK Dissolution Test System Unit is designed for the dissolution tests of solidpharmaceuticals according to the USP apparatus 1 and 2 and associated or related rules.

5.2 Instrument Features

§ Accurate stability of the mechanic

§ Chemical inert materials for the appropriate usage

§ Physical dimensions and tolerances according to the USP

§ Precision RPM control

§ Precision heat control

§ Easy access to all parts to be validated

§ No significant vibrations

5.3 Operational Specification

The Operational Specification is according to the individual Operation Manual.

5.4 Conformance Statement

The DISTEK Dissolution Test System Unit is designed and manufactured to a performance standardwhich meets or exceeds the specifications described for dissolution testing methods in USP GeneralChapter <711>.

CE Declared Compliance: EMC Directives 72/23/EEC, 89/336/EEC and 93/68/EEC via (or other codesas applicable) Standards EN 6100-3-2, EN 6100-3-3 and EN 61010-1, and further IEC 61326:2002,UL61010A-1.

5.5 System and Process Description

The DISTEK Dissolution Test System Unit is a lab bench top model with full accessibility to thedissolution vessels.

There is a timing, heat and RPM stirring control to perform the main issues of the dissolution test.

It provides reports for improved GLP documentation.

5.6 System Validation Conclusions

It is the conclusion from the USP demands to check the DISTEK Dissolution Test System Unit forphysical validation:




§ Generating no significant vibration during operation

§ Establishing precise temperature of the test media

§ Providing precise RPM control of the shafts connected with paddles or baskets

§ Precise spindle alignment

§ Precise centring of the shafts in the vessels

§ No significant wobble of the shafts

§ Precise height adjustment of the paddles or baskets in the vessels

§ Function of the system control (timing and printer interface)

There are Validation Tools from DISTEK available which should be used for the qualifications.

For the operation and handling of the DISTEK Dissolution Test System Unit use the OperationManual valid to the corresponding firmware version.

Note: We recommend you photocopy Pages from OQ to PQ of this Logbook and retain as templatesfor future 12-monthly calibration or 3- to 6-monthly performance tests on your DISTEK Dissolution TestSystem Unit.

5.7 Use of the Operational Qualification (OQ)

The installation, the transport and relocation or the repair of the DISTEK Dissolution Test System canhave influence on the specified parameters of the instrument. For this reason an physical OQ must beperformed. A physical OQ includes calibrations with adjustments of the parameters and performancetests without adjustments of the parameters. Therefore an OQ of the DISTEK Dissolution Test Systemaccording this Validation Logbook replaces a physical PQ.

5.8 Use of the Performance Qualification (PQ)

A physical PQ should be performed for a routine qualification in accordance with the In-TolerancePolicy. The chemical PQ with the USP calibrator tablets is not object of this Validation Logbook.

5.9 Recommended periods of OQ and PQ and preventive maintenance

It is recommended to perform every 12 months a preventive maintenance with PQ or OQ.

Note: We recommend photocopying pages from the OQ to the PQ of this Logbook. Retain them astemplates for the future qualifications / validations.

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6 Installation Qualification (IQ)

6.1 Customer Details and Reconciliation against Purchase Order

Attach Delivery Note or Invoice of the supplier.

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6.2 Identity of the Unit, Firmware and individual Operation ManualCOMMENTS DONE

Serial Number of the DISTEKDissolution Test System Unit

Firmware Revision

Operation Manual Version

6.3 Qualifying of the SiteCOMMENTS DONE

Suitable Bench Space, Surface andStability

Suitable Leveling

No Vibrations on the Bench

Correct Power Supply

6.4 Qualifying of the Cable and Tubing ConnectionsCOMMENTS DONE

Electrical Connections

Plumbing Connections

6.5 Installation Procedures

According to the individual Operation Manual:

COMMENTS DONE

Verified Installationaccording to the Operation Manual

Checked Principal Operationaccording to the Operation Manual

Attach protocols.

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6.6 Additional Comments

6.7 IQ CompletionInstallation Company:

Installation Engineer:

Installation Date:

Customer Representative:

Position/Job Title:

Department/Section:




7 Operational Qualification (OQ)

7.1 Level CheckDate Check Completed:

Performed By:

Approved By:

(1) Check the level on the vessel plate with a Carpenter’s Level as explained in the OperationManual.

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Level Check Passed Failed




7.2 Shaft and Vessel IDDate Identification Completed:

Performed By:

Approved By:

(1) Ensure that the system is fitted with stirring elements in all active shaft positions.

(2) Note the ID (Number or Serial Number).

Shaft Position Identification12345678

(3) Ensure that vessels are placed in all active vessel Positions and that rotational positions aremarked.

(4) Note the ID (Number or Serial Number).

Vessel Position Identification12345678

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7.3 Height Check BasketsDate Check Completed:

Performed By:

Approved By:

(1) The system is provided with height adjustment spacer to preset the height to the USPrequirements. Set the height adjustment spacer for the BASKETS.

(2) Use the DISTEK “Height Chek” instrument to measure the distance between the insidebottom of the vessel and the bottom of the Baskets for each position. The USP states that thedistance between the inside bottom of the vessel and the bottom of the stirring element ismaintained at 25 ± 2mm during the test.

(3) Document the results in the checklist below.

Check Results: Acceptance Criteria (USP) = 25 ± 2mm

Basket Position Height Deviation

1

2

3

4

5

6

7

8

Height Check Baskets Passed Failed

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7.4 Height Check PaddlesDate Check Completed:

Performed By:

Approved By:

(1) The system is provided with height adjustment spacer to preset the height to the USPrequirements. Set the height adjustment spacer for the PADDLES.

(2) Use the DISTEK “Height Chek” instrument to measure the distance between the insidebottom of the vessel and the bottom of the Paddles for each position. The USP states that thedistance between the inside bottom of the vessel and the bottom of the stirring element ismaintained at 25 ± 2mm during the test.


Check Results: Acceptance Criteria (USP) = 25 ± 2mm

Paddle Position Height Deviation

1

2

3

4

5

6

7

8

Height Check Paddles Passed Failed

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7.5 Center and Wobble CheckDate Check Completed:

Performed By:

Approved By:

(1) Raise the drive unit upwards.

(2) Lock the DISTEK “Center Chek” at the shaft of position 1, approximately 5cm above thestirring element (after lowering the drive unit into the working position the “Center Chek”should be approximately in the 500mL position in the half height of the vessel).

(3) Gently lower the drive head into the working position taking care not to break or damage thetip of the “Center Chek” (press the tip before it touches the vessel rim!). Lock the drive head.

(4) Start stirring at lowest velocity (25 RPM).

(5) Read the maximum and the minimum deflection on the instrument dial in ¼mm resolution.The USP states that the axis of the shaft positions is not more than 2mm at any point from thevertical axis of the vessels.

(6) Repeat step (1) to (5). Additionally watch the wobble of each shaft position. The shafts shouldrotate smoothly and without significant wobble.

(7) Document the results of the Center Check (results in ¼mm resolution!) and of the WobbleCheck in the checklist below.

Note: The Center Check is measuring the maximum and minimum deflection of the shaft or spindleposition versus the virtual vertical axis of the vessel. A maximal deviation of ± 2mm radius of thevessel axis will be measured by the Center Check with the distance of 4mm.

Note: The individual wobble during routine operation with an attached stirring element (paddle orbasket) has to be checked from the operator.

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Check Results: Acceptance Criteria (USP) = max. Deviation ± 2mm (or 4mm Distance absolute)No significant Wobble

Shaft Position MaximumDeflection

MinimumDeflection Distance Wobble

1

2

3

4

5

6

7

8

Center Check and Wobble Check Passed Failed

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7.6 RPM and Vibration CheckDate Check Completed:

Performed By:

Approved By:

(1) Place a piece of reflective tape on any of the shafts to be able to aim the light beam of thetachometer up on the tape. Alternatively using a contact type tachometer, bring the tip of thetachometer probe in contact with the extension at the top of the shaft.

(2) Set the unit to the required RPM of 50. Make a measurement as explained in the instructionsfor the use of the tachometer. The USP states that a used Speed Regulating Device allowsthe shaft rotation speed selected and maintained at the rate specified in the individualmonograph to be within ± 4%.

(3) Repeat the procedure explained in (2) for the required RPM of 100 and 150.

(4) Furthermore the USP states that no part of the assembly, including the environment in whichthe assembly is placed, contributes significant Vibration apart from the smoothly rotatingstirring elements.

(5) Document the results of the RPM Check and Vibration Check in the checklist below.

Note: All spindles turn with identical rotational velocity because the spindle’s drive is performedthrough one motor and one belt. Therefore the RPM measurement on anyone position will hold true forall positions. Nevertheless the synchronous and smooth motion of all spindles must be checked.

Note: Vibration from the environment was documented when the system has been installed.Nevertheless all type of vibration must be checked on this stage.

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Check Results: Acceptance Criteria (USP) = max. Deviation ± 4%; Synchronous and SmoothMotion; No significant Vibrations

RPMSet Point

RPMMeasurement Deviation Deviation % Synchronous

MotionSmoothMotion Vibration

50

100

150

RPM Check and Vibration Check Passed Failed

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7.7 Temperature CheckDate Check Completed:

Performed By:

Approved By:

(1) Ensure each vessel is filled with 900mL of DI water and covered with a vessel cover.

(2) Run a heating at 37°C and wait for final temperature stability in the vessels. The USP statesthat the water bath or heating jacket permit holding the temperature inside the vessels at37 ± 0.5ºC during the test and keeping the bath fluid in constant smooth motion.

(3) Measure the actual value of the temperature in each vessel using a calibrated TemperatureSensing Device (reference value) and simultaneously compare with the displayedtemperature value of each vessel (if available). The displayed temperature values shouldagree within ± 0.25°C with the reference values. Otherwise perform a calibration of the built inthermometer(s) according to the Operation Manual and add the calibration protocol. Repeatpoint (3).


Note: There are two facts to distinguish: first, the temperature calibration of the internalthermometer(s) indicated in comparison with the measured external temperature of the calibratedTemperature Sensing Device; second, the heating control for reaching and indicating internaltemperature. Specification covers both, matching of the external and internal temperature with settemperature.

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Check Results: Acceptance Criteria (USP) = ± 0.5°C within Set Point

Vessel No. Set Point DisplayedTemperature

MeasuredTemperature Max. Deviation

1

2

3

4

5

6

7

8

Temperature Probe —

Temperature Check Passed Failed

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7.8 System Control Check (Timing)Date Check Completed:

Performed By:

Approved By:

1) Ensure each vessel is filled with 900mL of DI water and covered with a vessel cover.

2) Check the time periods which are suitable for routine, e.g. 30 minutes. Measure the right timingwith simultaneous activation of a calibrated timer watch and confirmation at the unit. The USPstates that specimens are to be withdrawn only at the stated times within a tolerance of ± 2%, iftwo or more times are specified.

3) If available check the functionality of the sophisticated instrument operation (e.g. parametersettings, printer interface).

4) Document the results in the checklist below.

Note: There are two facts to distinguish: first, is the instrument specification of the timing, second, isthe performance of the operator’s sampling timing. Since the tasks have to be executed by the sameperson, the measurements depend on the precision of coordination. An acceptance criteria of ± 4sectakes the degree of difficulty into account to precisely coordinate all tasks.

Check Results: Acceptance Criteria (USP) = ±2% or ± 4sec

Test No. Test Description Set Pointof the Time Period

TimeMeasurement

Deviation

1

2

3

4

5

6 Instrument Functionality

System Control Check (Timing) Passed Failed

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7.9 Summary SheetAcceptance Criteria Performed Passed/Failed

7.1 Level Check —

7.2 Shaft and Vessel ID — —

7.3 Height Check Baskets 25 ± 2mm

7.4 Height Check Paddles 25 ± 2mm

7.5 Center and Wobble Check ± 2mm or 4mm abs.

7.6 RPM andVibration Check

± 4%Synchronous and Smooth Motion

No significant Vibrations

7.7 Temperature Check ± 0.5°C

7.8 System Control Check(Timing) ± 2% or ± 4sec

7.10 Calibration EquipmentType Serial No. Certificate No. Dated

Carpenter’s Level

Height Chek DISTEK

Center Chek DISTEK

RPM Chek DISTEK

Thermometer

Chronometer

Attach Calibration Certificates or indicative paper of instruments which are not originated from thecustomer.

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7.12 OQ CompletionQualification Company:

Qualification Engineer:

Qualification Date:


Position/Job Title:

Department/Section:




7.13 OQ RecordTest Date Due Date of the

next OQ TestPerformed By Approved By




7.14 Training Certificate Record

Attach the Certificate(s) of the person(s) executing the OQ.

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8 Performance Qualification (PQ)

8.1 USP Calibrator Tablet Test

This section has been left blank in preparation for the user documentation. Attach SOP for the PQTest and results there from.

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8.3 PQ CompletionQualification Company:

Qualification Engineer:

Qualification Date:


Position/Job Title:

Department/Section:




8.4 PQ Record

Please attach a copy of each PQ test report to this Record, every time the unit is checked.

Test Date Due Date of thenext PQ Test

Test Type Performed By Passed/Failed

Note: “Test Type” states which USP test programme has been performed.




9 Maintenance Qualification (MQ)

This section has been left blank in preparation for the local dealer documentation.




10 Service Record

Service Date Service Engineer Details Visit Purpose (see Note)

Note: The Service Record should provide a record of “unplanned” engineer visits, e.g. to carry outemergency breakdown repairs, thus “pre-planned” visits for calibration testing or preventativemaintenance should not be entered as they will be covered in section 6, Operational Test Record.




11 Operator Record

This section has been left blank in preparation for the user documentation.




12 Training Policy

This section has been left blank in preparation for the local dealer documentation.

dissolution test system validation · pdf filei agree that the iq, the oq and the pq...

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