Extended Edition. Version 2. IDIS EE Operation Qualification for Online Collection and Dilution and Measurement

Transcription

1 Extended Edition Version 2 IDIS EE Operation Qualification for Online Collection and Dilution and Measurement Revision 1.1 Part Number st May 2003

2 Document Authorisation The System Validation Team has reviewed these Installation Qualification Test Scripts and confirms that they meet the business and regulatory requirements of (Department name) (Company name) First Responsible Person Name Position Department Signature..... Date Second Responsible Person Name Position Department Signature..... Date IT Support Name Position Company/Department Signature..... Date Regulatory Support Name Position Company/Department Signature Date..... IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 2 of 86

3 Table of Contents 1 COMPANY & WARRANTY DETAILS ICALIS DATA SYSTEMS LTD, THE COMPANY OVERVIEW IDIS EE FUNCTIONALITY OPERATIONAL QUALIFICATION DETAILS SCOPE AUDIENCE ASSUMPTIONS, EXCLUSIONS, LIMITATIONS PERFORMING THE OPERATIONAL QUALIFICATION Roles and Responsibilities How to Perform the Test Scripts REFERENCES ROLES AND RESPONSIBILITIES Identification of Signatories IDIS EE SYSTEM ACCES S ADMINISTRATOR LOG ON SECURITY CHECK New User Logon and Password Change Access User Log On Password and Access User Password Expiry Check Automatic Log Off Time Check Configuring Signing Levels and Assigning Users MANUAL ACCESS TO CONFIGURED INSTRUMENTS Autosampler Configuration METHOD CONFIGURATION - FOR COLLECTION METHOD CONFIGURATION - FOR DILUTION METHOD CONFIGURATION - FOR INJECTION METHOD CONFIGURATION GENERAL PARAMETERS Autosampler Check Diluter Dispenser 1 Check Bath 1 Check Pump 1 Check Sampling Valve Check Media Selector Check Media Switcher 1 Check Media Switcher 2 Check RUN SEQUENCE TESTS RUN SEQUENCE CALCULATION TEST SCRIPT Objective Requirement Installing the Drivers for Single Component USP Methods I and II Creating a Single Component Calculation Method for USP I & II Performing the Calculation Test Post Editing Sampling Loss Correction Saving Post Edited Data Data Export Check...69 IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 3 of 86

4 9 SIGNING RECORDS Electronic Signing of Records Viewing and Signing Records Electronic Signing of Records Verifying User Signatures Electronic Signing of Records Final Signature Electronic Signing of Records Verifying User Signatures for all Levels AUDIT TRAIL VERIFICATION TEST EXECUTION NOTES AND SUMMARY LOG TEST EXECUTION NOTES OPERATIONAL QUALIFICATION SUMMARY LOG OPERATIONAL QUALIFICATION SIGN-OFF REVISION HISTORY AUTHORISATION OF MASTER FORM IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 4 of 86

5 1 Company & Warranty Details Company Name: Address : Contact Purchase O/N Invoice No. System Name IDIS EE Serial No. Installed by Print Name :. Signature :. Date :. Warranty and Support Details Date Installed... : Initial Warranty Period.. :.. to.. After Sales and Extended Warranty : IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 5 of 86

6 2 Icalis Data Systems Ltd, the Company Icalis Data Systems Ltd was established in The company s original business was developing and marketing software for instrument control and data processing, notably a contract with Shimadzu to deliver a front end for their Spectrofluorimeter and Densitometer. In the early nineties, the company launched its first tablet dissolution software under DOS. This product sold over 300 copies world wide in all the major Pharmaceutical companies In 1994, the company developed the specification for its IDIS EE software that is its major focus today. Icalis Data Systems Ltd is a wholly and privately owned UK company whose business focus is integrated systems, professional data management software which integrates laboratory instruments to deliver unique final solutions with LIMS. The company s current main product is its Dissolution software that is sold world wide through its international dealership. The company currently employs 12 persons at its development site in the UK, of which four personnel (two BSc Graduates and a Doctor in Biochemistry) are on full time development of the IDIS EE product. In addition to the software, Icalis also manufacture laboratory instruments including Pumps, Media Selectors for ph Change, Valve Selectors for multiplexing multiple baths to single detectors (including ph / Conductivity Electrode), Autosamplers, Fraction Collectors, Media Preparation Units and Fibre Optics Multiplexers. A range of other hardware and software products is planned. We also market a charge coupled device (CCD) array spectrometer for both research and process control markets. Icalis Data Systems Ltd international dealership is appointed by their ability to provide sound technical support and after sales service to the pharmaceutical industry. This network provides Icalis with sales, technical support and after sales service in nearly all the major industrial countries including the UK, France, Germany Switzerland, Benelux, Sweden, Canada as well as some far eastern countries. There are multiple installations of Icalis Data Systems Ltd software products in many of the largest pharmaceutical companies such as Novartis, GSK, Roche, Pfizer, Solvay, Schering to name but a few. Our future focus is to deliver a combination of software and hardware systems which can be configured to acquire data from most laboratory techniques. Keith Wilkinson Managing Director IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 6 of 86

7 3 Overview This document is intended to be used for on-site testing of the software for conformance to the specification described by Icalis Data Systems Ltd and to assist the user in conforming to the Pharmacopoeia validation requirements. This Operational Qualification is intended for use as a standard procedure to check the IDIS EE software setup and connectivity of the instrumentation. This document, together with the Installation Qualification document and Icalis Data Systems Ltd and our distributors technical support and knowledge of tablet testing are designed to assist you in meeting the requirements of Regulatory Authorities your laboratory deals with. The procedures and logging of the results from the tests make the validation process very easy to understand and implement. Keith Wilkinson Managing Director IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 7 of 86

8 4 IDIS EE Functionality The IDIS EE Dissolution software enables automatic on-line dissolution measurements to be made through control of various baths, pumps, auto-samplers and detectors. Data acquired from the detectors is processed to calculate the results in a suitable user specified format but mostly the Weight Content and %Dissolution of the product under test. The dissolution system set-up consists of a Dissolution bath conforming to the BP, EP, USP and other pharmacopoeia specification for tablet dissolution. Commonly USP apparatus I &II, III or apparatus IV, an appropriate pump, and detector (spectrophotometer etc.). The bath containing the dissolution media is heated at a constant temperature and possibly stirred (depending on the apparatus type) at a pre-set speed. Dissolution media from each vessel (usually 6 vessels) is pumped by a multi-channel pump either through to the detector where readings from the detector (i.e. Absorbance from a spectrophotometer) are taken at predefined Time Intervals set in the IDIS EE software. Alternatively the media from the Vessels can be pumped to a fraction collector where the analyst can use the fractions for HPLC or measure these fractions on a spectrophotometer. Or the media may be pumped to an XYZ auto-sampler where the samples can be taken and optionally diluted and read either in real time or after the dissolution test is completed automatically by the IDIS EE software. At the beginning of the experiment the IDIS EE software will control all instruments configured by the user for the experiment through RS232, GPIB IEEE or Output contact closure. Parameters set in the method are transferred to the appropriate instrument using a specific independent driver written by Icalis Data Systems Ltd for the instrument in question. These may include the wavelength for the spectrophotometer, or the rotation speed for the bath etc. In most cases if defined by the user, at the start of the experiment a reading is taken with blank media in all Cells in the spectrophotometer (baseline reading), and is subtracted from all subsequent readings to give the absolute reading of the substance in the cell. IDIS EE will then select each vessel in turn and read this offset baseline value. At the specified interval(s), readings are taken for each vessel and plotted graphically and displayed numerically in real time. Using the value of standard which is read at the beginning of the experiment, during the experiment at each interval or entered in the method, the drug content is calculated for all vessels in real time as a Weight Content or %Dissolution and displayed numerically or graphically. The individual or mean drug release for the six vessels, the statistics (mean, standard deviation, variance etc.) and the %Dissolution or the Weight Content can be selected to be displayed in real time. IDIS EE controls the timing functions at each sampling interval for the Staggered Time, the Tubing Delay Time, The Media Delay Time and the Cell Delay Time as specified by the operator. IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 8 of 86

9 5 Operational Qualification Details 5.1 Scope The enclosed procedures describe tests which can be carried out to verify that the IDIS EE software is operating correctly. The approach taken is to provide generic Test Scripts which, once executed, will identify any missing or non-operational components of a working system. These tests will check the effectiveness of the configured IDIS EE system to provide a compliant environment for the following functions; instrument control, data acquisition, result calculation, presentation and reporting of data and the secure management of information. This Operational Qualification is applicable to any installation of IDIS EE as either a standalone or a networked system. The complexity of each IDIS EE system may vary and many different instrument configurations are possible (1-4 Baths). This Operational Qualification allows for the diversity but will require the Tester and Reviewer to indicate which options and equipment are installed and hence which tests are to be executed. 5.2 Audience This document is intended for suitably qualified users who have purchased the IDIS EE system, Icalis Data Systems Ltd qualified staff, an appointed distributor or an experienced person appointed by the company to carry out these tests. 5.3 Assumptions, Exclusions, Limitations This Operational Qualification assumes that the installation, configuration and setup of the IDIS EE was carried out and tested by suitably qualified personnel. It is assumed that this Operational Qualification will be executed after the installation of the system, after performing the Installation Qualification, after the system has been configured with the laboratory equipment and tested but before live use in a regulated area. These Test Scripts can also be executed to periodically exercise the system or after a major reconfiguration but it is assumed that any errors, warning messages or cautions from any diagnostics or testing will be recorded and corrected before the Test Scripts are used. Prior to using these Test Scripts the laboratory equipment connected to the IDIS EE must have satisfactorily completed their respective Installation and Operational Qualifications and have current and documented maintenance programs in operation. The qualification of the computing service for a networked IDIS EE solution is excluded from this Operational Qualification. It is expected that the security, integrity, robustness and suitability of both the computer serving the application and the networking infrastructure is the responsibility of the computing service provider. This service should be demonstrated to be compliant and documented in a service level agreement between the computing service provider and the IDIS EE user personnel. IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 9 of 86

10 5.4 Performing the Operational Qualification The execution of this Operational Qualification requires the judgement and knowledge of suitably trained personnel and the careful documentation of each Test Script particularly in areas with multiple applications and laboratory equipment. All staff executing these Test Scripts should provide copies of suitable training or certification to append to the Operational Qualification document set Roles and Responsibilities A minimum of two people are required to perform this Operational Qualification, a tester executing the scripts and a reviewer to check that the data and conclusions drawn are correct and recorded accurately. The details of all personnel involved with the execution or review of the Operational Qualification must be entered in the Identification of Signatories table, Section The roles are defined as follows: Tester: Reviewer: Icalis Data Systems Ltd personnel or approved distributor, Trained and Authorised Users. Ideally an experienced user, familiar with dissolution testing How to Perform the Test Scripts To perform a Test Script read through prior to execution and ensure that the status of all equipment is as expected. Then follow the steps in the script annotating the actual results or a summary in the boxes provided. The tester should initial and date the individual steps and then the tester and reviewer should sign-off the script with initials and date. Test Scripts requiring information should be completed by the tester, checked by the reviewer and signed-off as above with initials and date. On completion of an individual Test Script, the tester deletes as appropriate the Passed / Failed statement at the end of each Test Script and then writes Pass, Fail or N/A in the appropriate box provided in the Operational Qualification Summary Log (Section 8.2) On completion of all the Test Scripts and the Summary Log, the tester signs the Operational Qualification Sign Off, Section 9. The reviewer then ensures that all data is correctly entered and collated, re-checks the scripts and confirms the conclusions of the tester and signs off the Operational Qualification, Section 9. It should be noted that some Test Scripts have an information row at the top of the table and this is to be filled as completely as possible to identify the laboratory components in use for the IDIS EE System in question. If the particular component is installed, then enter `YES` in the Installed box. If the component is not installed, then enter `N/A` in the Installed box IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 10 of 86

11 On completion of each Test Script the IDIS EE system should be returned to the status at the beginning of the test e.g. the Instrument Control dialogue should be closed to return the instrument to local control. If during the execution of an individual Test Script the procedure is suspended then an entry must be made in the Test s Log. If the whole procedure is stopped then an entry must be made in the Test s Log and a suitable statement defining the circumstances must be appended to the documentation set. The testing can be resumed providing the individual Test Script is not using either a timing component or setup from a previous test. Test resumption must also be recorded in the notes log. All unexpected results, anomalies, notes or errors should be recorded in the Test s Log and identified primarily by the test script number. As the incidents / notes occur within the execution of an individual Test Script they are allocated an integer number, starting at 1 and increasing by 1 for each incident / note. A full description of the incident / note and staff initials must be entered in the appropriate boxes. This will allow positive identification of any information relevant to the script and will help with possible problem escalation and or resolution. e.g. Test s Log Test Script No: s Log No: Description The first row of each test script has an Installed field. The tester must enter Yes or No as appropriate to indicate whether the instrument is installed and the script will be performed. If No is entered, only the signatures at the end of the script are required. Enter Yes in the Results As Expected column or No if an unexpected result is obtained. The tester must indicate which options are installed and hence which Test Scripts are to be executed. The Test Scripts deemed not appropriate must be marked as not applicable, N/A. All forms must be completed either by executing the tests and recording the results or marked as not applicable, N/A. Any changes to the Test Scripts content or text must be initialled, dated and a summary reported to Icalis Data Systems Ltd. Any notes or problems encountered during the execution of the Operational Qualification due to the construction or style of the documentation must be reported to Icalis Data Systems Ltd. IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 11 of 86

12 5.5 References The table below lists any reference documents or materials used for calibration which is referred to in this manual. Reference Title IDIS EE Installation and Instrument Setup manual Revision or Part Number IDIS EE User Manual Reference Materials Part Number Make Model Recalibration Date Calibrated Stopwatch Holmium Oxide Filter N/A Calculation Text Files : N/A indicates Not Applicable and this information is not required. IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 12 of 86

13 5.6 Roles and Responsibilities A minimum of one tester and one reviewer is required to execute this Operational Qualification Identification of Signatories All testers and reviewers must enter their details in the table below. Name Company / Position Signature Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 13 of 86

14 6 IDIS EE System Access These check scripts will check the IDIS EE software for access security functionality. These checks will form some of the requirements for 21 CRF Part 11 compliance. Other checks in this document (i.e., signing of electronic records) will add additional testing to comply with the 21 CFR Part Administrator Log on Security Check Objectives To show that the administrator can log onto to the Administration group with the correct password only. Double click the IDIS EE icon from the Windows desktop, or from the Start up program menu. Select User on the toolbar IDIS EE Shell window appears. A drop-down menu appears Log Select Administration from the drop-down menu Enter the name of the current IDIS EE system administrator in the User Name field. Click the OK button without entering a password. Select OK. Enter an incorrect password in the password field. An Administration Log On window appears. User Name, Password and Group fields are displayed The name entered is displayed correctly. Access to the IDIS Application is denied. An error message is displayed. The name entered is displayed correctly. Access to the IDIS Application is denied. An error message is displayed. Select OK. password. Enter the correct The password is displayed as xxxxx as it is being typed. A Log On Accepted message is displayed with the administrators Full Name, Group and Level The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 14 of 86

15 6.1.1 New User Logon and Password Change Access Objectives To show that a new user created must change their password when they first log on to the IDIS application and the password must be different than that entered previously.. Expected? Right mouse click on the group name created when the database was first installed Right mouse click on the Group and select Edit Group Details Set the Minimum Password Length to 6 followed by OK Select Add New User Enter a new users log on name, Keith, full name, Keith Townsend and password keith Enter a password and confirmation keith1 Select OK Select User, Application and OK. Enter the user name, Keith and password keith1 and click OK Drop down menu appears The group Details dialogue appears An Add A New User dialogue box appears A dialogue box appears indicating the password entry is too short All entries are accepted and the new users log on name should appear under Users The Application Log On box appears The password is displayed as xxxxxx as it is being typed. The Log On Accepted prompt appears Press OK An Enter New Password dialogue appears Enter the password keith1, a new password keith1 and confirmation password keith1. Select OK Select OK and enter the password keith1, a new password keitht and confirmation password keitht. Select OK Select the Administrator Group and log on as the administrator Right mouse click on the Group and select Edit Group Details The password is displayed as xxxxxx as it is being typed. An error is displayed warning the user that the password has already been used The Application Level access appears The group Details dialogue appears Set the Minimum Password Length to 4 followed by OK The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date Initial s Log IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 15 of 86

16 6.1.2 User Log On Password and Access Objectives A user must enter their correct name and password to gain access to the IDIS EE application. If the number of tries and attempts are exceeded, the workstation is locked. Expected? Log Log on as Administrator onto Administration Level. Create and select a Group called Validation Expand the group folder; select Group Access Rights followed by Data. Disable all the Post Edit Rights Disable Save Post Edit Data The group specified is created The access rights can be deselected Select Global Settings. Enable the Audit Trail Select the Log On Tab Enable the number of Tries and set the Number of Tries to 5. The Enable Button is switched on The Log On Tab dialogue is displayed Entries specified are accepted Enable the number of Attempts and set Number of Attempts to 2 and select OK Select the Validation Group and add the New User John Smith with Log On Name John and Password john Log Off from the Administration Group Select User on the toolbar Entries specified are accepted The entries specified are accepted The IDIS shell Window appears A drop-down menu appears Select Application from the drop-down menu and Validation Group Enter the User Name John Enter the Password john Select OK. Enter the current password as john and the new password as letmein. Enter letmein again for the confirmation Select OK. Select User on the toolbar Select Log Off An Application Log On window appears. The name entered is displayed correctly. Password is echoed as it is typed as xxxx A Log On Accepted message is displayed An Enter New Password dialogue box appears Entries are accepted The Application Level Window appears. A drop-down menu appears. Application option is greyed out IDIS Shell Window appears /continued IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 16 of 86

17 User Log On Password and Access continued 1 Select Application from the dropdown menu An Application Log On window appears. Enter the User Name John The name entered is displayed correctly. Select the Validation Group Log Select the OK button without entering a password. Select OK. Enter the User Name John and enter the password as John Select OK. Enter the User Name John and enter the password as JohnS Select OK. Enter the User Name John and enter the password as John Smith Select OK. Enter the User Name John and enter the password as JSmith Select OK. Select OK. Select User on the toolbar Select Application from the dropdown menu Enter the User Name John and enter the password as John S Select OK. Enter the User Name John and enter the password as J Smith Select OK. Enter the User Name John and enter the password as Smith Select OK. Enter the User Name John and enter the password as JohnSmith /continued A Log On Failure message is displayed A Log On Failure message is displayed A Log On Failure message is displayed A Log On Failure message is displayed A Log On Failure message is displayed An Attempt Failure prompt appears IDIS Shell Window appears A drop-down menu appears An Application Log On window appears. A Log On Failure message is displayed A Log On Failure message is displayed A Log On Failure message is displayed A Log On Failure message is displayed IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 17 of 86

18 User Log On Password and Access continued 2 Select OK. Log Enter the User Name John and enter A Log On Failure message is displayed the password as SmithJohn Select OK. Administrator Assistance prompt appears. Select OK. Select User on the toolbar Select Administration Enter Administrators User Name and Password Select OK Select OK Select OK A drop-down menu appears with Administration as the only option available An Administration Logon dialogue box appears Entries are accepted A Prompt appears stating that the system has been locked and an entry will be added to the Audit Trail Log On Accepted message is displayed The Administrative Window appears Select User on the toolbar Re-enable all the post edit rights for the Validation Group A drop-down menu appears with all levels available The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 18 of 86

19 6.1.3 User Password Expiry Check Objectives To show that when an expiry date is set, after this time, the User is prompted to enter a new password. Log on as Administrator onto Administration Level No errors occur Log Select Global Settings Display the Password Expiry and Reuse Tab Set the Password Expiry to 1 day The Expiry Time is shown in days No errors occur Log Off immediately No errors occur Reset the System Clock by advancing it by 1 day Log on as user John in Validation Group with the password letmein No errors occur Log On Accepted Select OK Enter the current password as letmein and the new password as tester. Enter tester again for the confirmation An Enter New Password dialogue box appears with a Password has expired message Entries are accepted Select OK. The Application Level Window appears. Reset the Password Expiry to 99 days Reset the System Clock to the correct date The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 19 of 86

20 6.1.4 Automatic Log Off Time Check Objectives To show that when the keyboard and mouse is not used for a specific length of time, the user is automatically logged off from each level. It is important that the mouse does not move for the following tests and it may be necessary to turn the mouse upside down to prevent small movements. Log Log on as Administrator onto Administration Level Select Global Settings and Log Off Times tab Set all the Log Off Levels to 2 minutes followed by OK Have a Stopwatch at hand and without touching the keyboard or mouse, start the stopwatch Log into the Device Management level Without touching the keyboard or mouse, start the stopwatch Log into the Approval level At 2 minutes ±10 secs, the user should be logged out of this level No errors occur At 2 minutes ±10 secs, the user should be logged out of this level No errors occur Without touching the keyboard or mouse, start the stopwatch Log into the Application level At 2 minutes ±10 secs, the user should be logged out of this level No errors occur Without touching the keyboard or mouse, start the stopwatch Reset all log off times to the previous settings or to 22 hrs for all levels. At 2 minutes ±10 secs, the user should be logged out of this level The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 20 of 86

21 6.1.5 Configuring Signing Levels and Assigning Users Objectives Signing levels can be configured and different users assigned to each level Log on as Administrator onto Administration Level Add User Keith Townsend to the Validation Group if he is not already added Right mouse click on the Validation Group and select Group Signing from the menu which appears Proceed as described in the Administration Manual in the section Electronic Signature Access and configure two signing Levels: - Analyst and Supervisor for Data signing Add User John Smith to the Analyst level Add User Keith Townsend to the Supervisor level Add Analyst Sign Off and Tested by for the Meaning and Singer Action respectively for the Analyst signing level Add Approve d by and Checked and Verified Results for the Signer Action and Meaning respectively for the Supervisor signing level Select Settings followed by Electronic Signing and set the signing order as follows Signer Action Signer Date & Time - Meaning Log out of the Administration level No errors occur User Keith Townsend is in the Validation Group Group Signing dialogue appears Signing levels specified are created User is added to Analyst signing level User is added to Supervisor signing level Analyst labels are created for Signer Action and Meaning Supervisor labels are created for Signer Action and Meaning Signing order is set No errors occur Log The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 21 of 86

22 7 Manual Access to Configured Instruments This section of the Operational Qualification will check that those devices configured for the method can be selected and controlled manually from the IDISEE application window. Please note that some of these tests were performed as part of the Installation Qualification but this needs to be performed, as this is a function the user accesses in the process of using IDIS routinely. Requirement The Instruments configured for the method should appear on the Icon Bar and also on the Instrument Connection View. All devices should respond to parameters being set by the user from the appropriate instrument Control dialogue. IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 22 of 86

23 7.1.1 Autosampler Configuration For this test, the Autosampler should have been installed as described in the IDIS EE Installation manual. Log On to the Device Management The Device management is accessed Log Set the Autosampler to remote control if required. Right mouse click on the Autosampler icon in the Device Management and select Initialise. Right mouse click on the Autosampler icon again and select Probe Settings. Enter appropriate values for the X, Y and Z numeric fields for the Wash Position Select the Go to Position button. Select Finish and Save Right mouse click on the Autosampler icon again and select Physical Rack Settings. Select the Create Rack button and enter Rack 1 as the name and press Next. Enter appropriate values for the X, Y and Z numeric fields for the Start Position. Select the Go to Position button. Select Next and Repeat the steps above to position the probe at the End Position Select the Go to Position button. Enter 6 or more for the Number of Y Enter 1 only for the Number of X Create a second Rack, labelled Rack 2 Define the Start position and select the Go to Position button The Initialise prompt should appear. The Probe Settings dialogue is displayed. The Probe is configured as specified. The Autosampler probe moves to the X, Y and Z co-ordinates entered The Physical Rack Settings dialogue is displayed. The Physical Rack Dialogue box becomes active. The values entered are accepted The Autosampler probe moves to the X, Y and Z co-ordinates entered The values entered are accepted The Autosampler probe moves to the X, Y and Z co-ordinates entered Value entered are accepted Values entered are accepted The input is accepted. The Autosampler probe moves to the X, Y and Z co-ordinates entered IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 23 of 86

24 Autosampler Configuration continued Define the End position and select the Go to Position button. Enter 6 for the Number of Y The Autosampler probe moves to the X, Y and Z co-ordinates entered Value entered are accepted Log Enter 4 or greater for the Number of X Create a second Rack, labelled Rack 3 destined for Injection Define the Start position and select the Go to Position button Define the End position to be the same as the start position and select the Go to Position button. Enter 1 only for the Number of Y Enter 1 only for the Number of X Select Finish and OK Select the Save icon from the toolbar. Right mouse click on the Autosampler icon again and select the Probe Settings tab and Next. Select Next Select Finish Select the Save icon from the toolbar. Select OK Right mouse click on the Autosampler icon again and select the Logical Rack. Create a Logical Rack and labelled as Collection Rack Assign the Physical Rack, Rack 1 created above to this Logical Rack Select Next. Enter the Z values in the Aspiration Depth and Dispense Depth numeric fields. Select Finish Create a second Logical Rack, labelled as Storage Rack Values entered are accepted The input is accepted. The Autosampler probe moves to the X, Y and Z co-ordinates entered The Autosampler probe should be at the same position as the Start position. Value entered are accepted Values entered are accepted The Probe Settings dialogue box closes. The Probe Settings dialogue box is displayed. The Probe settings dialogue appears The Probe Wash settings previously entered should appear. No error messages are displayed. The Logical Rack Setup dialogue box is displayed. The rack named is created The Rack assigned is created. The X and Y Start Positions values are the same as those defined for the Start Position for the Physical Rack named Collection Rack. The values entered are accepted. The input is accepted. IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 24 of 86

25 Add the Physical Rack, Rack 2, to the No error messages are displayed. Logical Storage Rack. Select the GoTo Position button. The Autosampler probe moves to the X,Y and Z values entered. Enter the Z values in the Aspiration The input is accepted. Depth and Dispense Depth numeric fields Create a third Logical Rack, labelled as The input is accepted. Injection Rack Add the Physical Rack, Rack 3, to the No error messages are displayed. Logical Injection Rack. Select the GoTo Position button. The Autosampler probe moves to the X,Y and Z values entered. Enter the Z values in the Aspiration The input is accepted. Depth and Dispense Depth numeric fields Close and Save the rack settings Log The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 25 of 86

26 7.2 Method Configuration - for Collection Load the IDIS EE Application and login as a user. Make sure that the Diluter has been configured in the Device Management with a 5ml Syringe. Log No: If this is not the case scale the volumes up or down appropriately below and set the speed so the timings correspond to those set. Syringe Volume Configured (ml): Make sure that the Source and Destination racks have been configured before proceeding. Select a New Method template Select the following so that they appear on the Instrument Connection View. The Bath, Sampling Pump, Autosampler and Diluter. Add 6 Vessels to the Bath The IDIS method view appears All instruments specified appears on the Instrument Connection View The Vessels should appear Label the Vessels as Sample 1 to Sample 6 respectively. Link Sample 1 from Vessels 1 to the Sampling pump and from the Sampling pump to position 1 on the Collection Rack on the Autosampler. Link Sample 1 from Autosampler s Needle to one end of the Diluter. Repeat for Samples 2-6 using Vessels 2 to 6 respectively and ensure that all Samples are connected individually from the Autosampler Needle to one end of the Diluter. Add another Vessel close to the Diluter and configure this as a Media Connect this Vessel to the other end (to the opposite end used for the Samples link) of the Diluter The vessels are labelled as specified The links appears as specified Samples 2 to 6 are linked as specified The Vessel is configured as specified The link appears as specified IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 26 of 86

27 Method Configuration - for Collection Continued Leave the Bath Properties set to the default settings. Right mouse click on the Sampling Pump and set its Properties to Before and After. Set the Before Reading Direction to Forward, the Speed to 40 rpm, and the On Time to 90 sec. Or 15 mls at 10 mls/min for a Metering Pump Set the After Reading Direction to Reverse, Speed to 60 rpm, the On Time to 75 sec. Or 12mls at 10 mls/min Close the Pump Dialogue. Right mouse click on the Diluter, select Properties. Set the Diluter option to be Controlled by Sampler Select the Diluter Priming Tab and set the Priming Volume to be 5000 µl, Flow Rate 500 µls -1 and 2 Primes Right mouse click on the Autosampler, select Properties followed by Collection Properties. Select Do sample Collection and Collection Rack for the Source Rack and a Storage Rack for the Destination Rack Select Next and Wash Between Samples and set the Wash Volume to 2500 µl, 500 µls -1 for the Flow Rate and 1 for the Number of Washes. Set the Wash port Depth for Dispense Depth. Select Next and set 500 µls -1 for the Dispense Flow Rate and the Wash Dispense Depth for the Dispense Depth. Select Next and set 20 µl for the Pre Sample Air Gap, 500 µls -1 for the Aspiration Flow Rate and the Dispense Depth to 0. Select Next and set 2000 µl for the Sample Volume, 500 µls -1 for the Aspiration Rate and the Dispense Depth for the rack selected for Storage Rack The entries specified are accepted. Entries are accepted. The Pump Dialogue closes The Diluter Dialogue Properties appears The entry specified is accepted. The entries specified are accepted. The Collection dialogue appears The entries specified are accepted. The entries specified are accepted. The entries specified are accepted. The entries specified are accepted. The entries specified are accepted. Log No: IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 27 of 86

28 Method Configuration - for Collection Continued Select Next and Next to skip the settings for the Post Sample Air Gap Select Next and set 500 µls -1 for the Dispense Flow Rate and the Sample Dispense Depth to the values for the Storage Rack. Select Finish Post Sample Air Gap appeared after the first Next The entry specified is accepted. The Collection dialogue should close Log No: The IDIS EE System has Passed / Failed * this Test Script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 28 of 86

29 7.3 Method Configuration - for Dilution Right mouse click on the Autosampler, select Properties followed by Sample Assignment Select the Storage Rack for the Destination Source Rack name and enter 1 for the Assigned Tube Number Right mouse click on the Autosampler, select Properties followed by Sample Processing Properties Select Rack Dilution The Sample Assignment dialogue appears The Sample Processing Properties dialogue appears Rack Dilution is selected Log No: Enter a Dilution of 1 in 2 and Label this Dilution Sample Dilution 1 in 2 Select Properties and enter the Rack selected for the Sample Assignment above. Enter 13 for the Start Tube Number. Select Next and select Wash Between Samples and set the Wash Volume to 1000 µl, 500 µls -1 for the Flow Rate and 1 for the Number of Washes. Set the Wash port Depth for Aspiration Depth. Set Next and set the Wash Dispense Depth to the values for the Wash port. Set 500 µls -1 for the Dispense Flow Rate Select Next and set 20 µl for the Pre Sample Air Gap, 500 µls -1 for the Aspiration Rate and the Dispense Depth to 0. Select Next and set 1000 µl for the Sample Volume, 500 µls -1 for the Aspiration Rate and the Dispense Depth for the Storage Rack. Select Next and Next to skip the settings for the Post Sample Air Gap Set the Sample Dispense Depth to the values for the Sample Assignment Rack. Set 500 µls -1 for the Dispense Rate. The entries specified are accepted. The entries specified are accepted. The entries specified are accepted. The entries specified are accepted. The entries specified are accepted. Post Sample Air Gap appeared after the first Next The entry specified is accepted. /continued IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 29 of 86

30 Method Configuration - for Dilution continued Select Next and enable Perform Mixing Enter 25 µl for the Air Aspiration Volume, 800 µls -1 for the Aspiration Rate and 0 for the Aspiration Depth. Select Next and enter 1000 µl for the Aspiration Volume, 700 µls -1 for the Aspiration Rate and the Aspiration Depth for the rack selected for the Sample Assignment Rack Enter 2 for the number of Mixes and 0 for the Mix Delay Time Enter 500 µls -1 for the Dispense Rate. Set the Dispense Depth to the maximum Depth for the Sample Destination Rack. Select Finish Select OK to close the Sample Processing Settings Dialogue. Save the method The Perform Mixing options are enabled The Sample Processing Properties dialogue should close. Log No: The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 30 of 86

31 7.4 Method Configuration - for Injection Right mouse click on the Autosampler, select Properties followed by Injection Properties Select the Injection Rack for the Destination Rack name and enter 1 for the Start Tube Number Select Next and select Wash Between Samples and set the Wash Volume to 500 µl, 600 µls -1 for the Flow Rate and 1 for the Number of Washes. Set the Wash port Depth to the depth for the Probe Wash position. Set Next and set the Wash Dispense Depth to the values for the Wash port. Set 600 µls -1 for the Dispense Flow Rate Select Next and set 20 µl for the Pre Sample Air Gap, 500 µls -1 for the Aspiration Rate and the Dispense Depth to 0. Select Next and set 1500 µl for the Sample Volume, 600 µls -1 for the Aspiration Rate and the Aspiration Depth for the Storage Rack. Select Next and Next to skip the settings for the Post Sample Air Gap Select Next and set 1500 µl for the Dispense Volume, 600 µls -1 for the Dispense Rate and the Dispense Depth for the Injection Rack. Select Next, Next and Finish The Sample Assignment dialogue appears The entries specified are accepted. The entries specified are accepted. The entries specified are accepted. The entries specified are accepted. Post Sample Air Gap appeared after the first Next The entries specified are accepted. Log No: The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 31 of 86

32 7.5 Method Configuration General Parameters Expected From the Windows Menu Bar, Select Parameters then Labels Enter System 1 OQ for the Product Name. Close the Labels dialogue box. Method Label dialogue box appears Log No: Select Parameters then Calculation Deselect Baseline Correction Select Ok to close the Calculations dialogue box. Select Parameters then Run Options Set Time Zero option to Read Values Select OK to close the Run Options dialogue box. Select Parameters then Sections Right mouse click on Section 1 then select Properties Insert 1 Readings and a 11 minute interval Set the Bath Stirrers to 100 rpm and the Temperatures to 37 Set the Equilibrate Temperatures In Vessels to 37 and the Tolerance to 0.5 Select Next and Finish Right mouse click on Group One and select Properties Select Next until the dialogue Reading Sequence Run Readings appears Add all 6 samples to the Reading Sequence Select Next Select Next and drag the Sample Dilution 1 in 2 onto the Sample Dilution Assignment Select next until Finish appears then Finish Calculations dialogue box appears Baseline Correction is deselected Run Options dialogue box appears Entry accepted Sections dialogue box appears Method Section Settings dialogue box appears The Values entered are accepted The Values entered are accepted Group One Property dialogue appears Samples are configured The Post Run Test Control dialogue should appear Sample Dilution 1 in 2 was added to the Sample Dilution Assignment IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 32 of 86

33 Expected Select OK to close the Sections dialogue The Run Setup Dialogue appears again The Sections dialogue closes Log No: Select File then Save to save the method Close all windows Log out of the current group The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 33 of 86

34 7.5.1 Autosampler Check Expected Log on in Application, Validation group Log No: Load the method created above Select the Autosampler. Right mouse click. And select Control. Initialise the Autosampler Select the Storage Rack Set Tube to number 14 and select Go To Position Select Go To Wash Position Close the Autosampler Control dialogue The method loads and all instruments configured appears in the Instrument Connection View The Control dialogue appears The Initialisation prompt appears The Collection Rack and Storage Rack defined earlier should appear The Storage Rack is highlighted The probe should move to position 14 The probe should move to the Wash Position previously defined The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 34 of 86

35 7.5.2 Diluter Dispenser 1 Check If the Pump is not installed then record N/A in the Installed Box below in the first column of this form. Installed: Asset No: Make: Serial No: Ensure that the Diluter Dispenser is connected with the appropriate cable to the selected port. Manually switch on the Device and set to remote control. Right mouse click on the Dilutor Dispenser symbol on the Instrument Connection view. Select Control Select Initialise. For a Dual Syringe repeat the following for both syringes Set the Aspirate and Dispense volumes to maximum and the Flow Rate to 300. Set the Aspirate Valve to Left and the Dispense Valve to Right. Aspirate and Dispense to confirm the correct valve positions. Repeat but with the Aspirate Valve to the Right and the Dispense Valve left Set the Aspirate and Dispense volumes to 50% of the maximum Using deionised water aspirate and dispense 6 aliquots and weigh these to 2 decimal places. 5-item dialogue box appears. The Syringe or Diluter Control dialogue box appears. The Device Initialised prompt appears. Sample Aspirates through the Left Valve and Dispenses though the Right Valve Sample Aspirates through the Right Valve and Dispenses though the Left Valve Weights: 1: 2: 3: 4: 5: 6: Log The calculated % Deviation should be within ± 2% % Deviation = [(100 (A./Expected vol) x 100)] Average = =A % Deviation = IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 35 of 86

36 Diluter Dispenser 1 Operational Check (continued 1) Set the Aspirate and Dispense volumes to 100% of the maximum Using deionised water aspirate and dispense 6 aliquots and weigh these to 3 decimal places. Weights: 1: 2: 3: 4: 5: 6: Log The calculated % Deviation should be within ± 2% % Deviation = [(100 (A./Expected vol) x 100)] Average = =A % Deviation = The IDIS EE System Passed / Failed * this check script. (* Delete as appropriate) Tester (initials) Date Reviewer (initials) Date IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 36 of 86

37 7.5.3 Bath 1 Check If the Bath is not installed then record N/A in the Installed Box below in the first column of this form. If Bath 1 does not have the capability to set any of the following, record N/A for the Results As i) View the Temperature ii) Head Movement iii) Sampling Arm iv) Multiple Probes Installed: Asset No: Make: Serial No: Load the method System 1 OQ Ensure that Bath is connected with the appropriate cable to the selected port. Manually switch off the Stirrers and Temperature Control for Bath (do not switch off at the mains supply), and then switch to Remote Control if required. Right mouse click on the Bath Symbol on the Device Connection View Select Control Select Initialise from the Bath Control dialogue Select OK With the Default Speed set at 50 rpm, select Set Speed Select Stirrer On Select Stirrer Off The instruments configured should appear Bath Stirrer should turn off and the Heater should stop. A menu item appears The Bath Control dialogue appears. The Device Initialised prompt appears. The prompt should disappear The Set Speed button should grey out Bath Stirrer should turn on at 50 RPM The Bath stirrer should stop Log Enter a speed to 75 and select Set Speed Select Stirrer On Select Stirrer Off The Set Speed button should grey out Bath Stirrer should turn on at 75 RPM The Bath stirrer should stop Select the Temperature Tab. Set the Temperature to 2 C below the current bath temperature and select the Set Temp. button The bath temperature dialogue should appear The Set Temp button should grey out IDIS EE V2 OQ Online Collection Dilution and Measurement 3 Distributors Copy Page 37 of 86