Agilent ChemStation Plus January 2003 Specifications General Description This document provides specifications for Agilent ChemStore C/S, Agilent ChemStation Plus Security Pack, Agilent ChemAccess C/S Agilent ChemStation Plus Method Validation Pack, which are part of the Agilent ChemStation Plus family. With the Agilent ChemStation Plus family you need only purchase the features needed.
1. Agilent ChemStore C/S Product Description Agilent ChemStore C/S is a scalable in-process chromatographic database for Agilent ChemStations. It provides a means to easily organize, review and approve analytical data based on study and sample information. Agilent ChemStore C/S supports the users' data review process offering statistically result summaries, flexible control charts, cross-sample reports and documented data archiving and restoring.
Based on standard database features, Agilent ChemStore C/S offers functionality which focuses on the user’s needs for fast, secure and traceable handling of chromatographic data: • User-defined or automated transfer of selected data from the Agilent ChemStation into the Agilent ChemStore C/S database. • Define, edit and manage “studies” as the underlying data storage format. • Manage or restrict data access in studies by assigning study access only to authorized users.
Agilent ChemStore C/S—System Requirements 1. Agilent ChemStore C/S standalone Hardware requirements The following list shows the minimum hardware requirements for this application: • 400-MHz Pentium II (Pentium IV recommend) • 4 GByte of free hard disk space • 96 MB RAM for single ChemStation instrument. 128 MB is recommended for best performance, for Windows 2000 the minimum requirement is 128 MB.
2. Agilent ChemStore C/S server Server hardware requirements Agilent has optimized the perforOracle® database system recommended to use a high speed dual processor system with sufficient RAM.
vary based on the size of the database selected at installation time and the number of concurrent connections (the number of active instruments acquiring samples to the database and Agilent ChemStore C/S review clients) and the backup requirements for the server database. Table 2 shows three recommended server configurations.
Note: The custom database configuration must be planned as a project with Agilent database consulting specialists prior to system installation. The size of the Agilent ChemStore C/S database is based on an Agilent ChemStore C/S system which has an average distribution of all Agilent ChemStation 2D and 3D techniques. Also, all Store in Addition checkboxes are enabled for all studies, as shown in figure 1.
Agilent ChemStore C/S — Working with Agilent ChemStore C/S 1. Data transfer The Agilent ChemStation Plus concept consists of different software components designed for the various tasks in the chromatographic laboratory. The Agilent ChemStation manages data acquisition and data analysis, and the Agilent ChemStore C/S database offers advanced data and result management along with additional sample information management such as data organization, result approval, and archiving.
that are assigned to the study. Users must be assigned to a study in order to review study data or spool data into the study. The amount of result and meta data that is stored in the Agilent ChemStore C/S database is defined on a per study basis. For example, the transfer of a set of results may also include the raw data, methods and sequence file used to produce those results. Custom fields allow additional information fields to be linked to each set of results (“run”).
ChemStore spooler – Managing data transfer from Agilent ChemStation to Agilent ChemStore C/S To ensure optimum performance of the Agilent ChemStation, a background spooler takes care of a secure result transfer from the Agilent ChemStation data into the Agilent ChemStore C/S database.
Performing statistics calculations The user may optionally select to have statistical calculations performed on the (numerical) data which is being reviewed, as shown in figure 5. This can be achieved using summary statistics that calculates statistical values based on a single column of numerical values.
Agilent ChemStore C/S — Reporting Agilent ChemStore C/S offers a powerful report generator enabling users to easily create and generate final summary reports. The preview function helps to interactively develop the desired report without requiring test printouts. Agilent ChemStore C/S comes with a set of built-in templates to cover the most common needs for summary reporting. These templates can be used as a starting point to build your own customized reports.
Agilent ChemStore C/S — User Interface The Agilent ChemStore C/S review client offers the user two main “toolkits”: data review and database administration. Sample and compound review Within the data review toolkit, the user has a choice of whether to see data organized by analysis (also referred to as “run” or “sample”) or by compound. Chromatogram/spectrum presentation Figure 8 is an example of a chart contained in the display area. Here, the display area can contain both graphics and a table.
Agilent ChemStore C/S — Database Administration, Backup and Recovery web-based application that can be run from any PC on the network. The review client provides the The Admin Client performs the graphical user interface (GUI) following main tasks on the server through which the user can accomdatabase using a service running plish the following administrative on the server. tasks. Although the capabilities of • Schedule archive, dearchive the entry-level and client/server and delete operations.
automated archival is restricted to 10. Each archive query is stored under a unique user-defined name and can be executed based on a configurable time interval (per query), for example, daily, weekly, monthly or in conjunction with a counter such as every x days. A test functions allows the user to obtain information on the number of runs that the query returns at the moment with the given query condition. For each archive query the name and path for the archive unit have to be specified.
Agilent ChemStore C/S — Product Options and Configurations Standalone version The complete Agilent ChemStore C/S standalone software is provided on the Agilent ChemStation Plus CD-ROM as described in table 6a. Agilent ChemStore C/S server The Agilent ChemStore C/S server product includes the ChemStation Plus CD-ROM and Oracle 8i revision 8.17 software on a separate CD-ROM offering one Oracle standard edition license.
2.
Working with Agilent ChemAccess C/S Data storage and organization Agilent ChemAccess C/S enables the Agilent ChemStation results (raw data, methods and sequences) to be securely stored on the Agilent ChemAccess Windows NT server. The results can be transferred automatically at the end of each run or interactively through the data analysis view of the Agilent ChemStation.
Server hardware requirements Server software requirements Agilent ChemAccess C/S supports up to 15 “concurrent” Agilent ChemAccess clients, where concurrent is defined as a client connected to the Agilent ChemAccess C/S server which either transfers result data from the Agilent ChemStation to the server for data storage or performs remote real time plot. Recommended server configurations are listed in table 7. • Windows NT 4.
3. Agilent ChemStation Plus Security Pack Product Description The ChemStation Plus Security Pack is a module of the Agilent ChemStation Plus Series designed to support the requirements of 21 CFR Part 11. In the Agilent ChemStation the ChemStation Plus Security Pack modifies data analysis and provides advanced data management with regard to supporting the requirements for electronic records. It also offers a procedure to sign off runs with an electronic signature.
cation lock to lock the current ChemStation session and avoid any unauthorized access to the ChemStation application. • A completely revised ChemStation operator access level which allows operating the entire application as ChemStation operator. • A modified batch review interface providing an automated user-independent data versioning with detailed audittrails for all modifications. • Complete change control documentation for methods and manual events.
Working with ChemStation Plus Security Pack Result management The ChemStation Plus Security Pack is designed to store ChemStation data in a relational database by transferring it as a post-data analysis spooling job to the database. The ChemStore C/S ODBC spooler is a proprietary tool managing the transfer and protecting data against loss, modification or damage in case of transfer problems or network errors.
Configuration and data protection using Windows security features For security reasons, a user must be a member of the Windows user group Administrators to access the configuration of the ChemStation Plus Security Pack. It restricts access to all data directories on the local PC with important information using the Windows users group privileges.
ChemStation Plus Security Pack — User Management and Application Security User management and ChemStation Plus Security Pack user access rights which should be enabled manually before leaving the PC unattended, e.g. during a break or shift change, and Security Pack provides a fully inte- • for enhanced security a timegrated user management that is based automated lock of the independent of the Windows opersession for other periods of ating system.
ChemStation Plus Security Pack — Data Integrity, Automated Result Versioning and Data Reanalysis Data integrity The Security Pack maintains full data integrity by storing all results along with the raw and meta data in a relational database as shown in figure 12. Result revision management Daily work in the analytical laboratory often requires sample reanalysis.
User-independent, automated result version management The data storage includes an application controlled version management that is based on the creation of a result reference file. Prior to reprocessing, the application software creates a binary result registry file called save_sec.reg for each file. This save_sec register is stored along with the raw data. It includes all numeric results of the current result revision in a binary format, such as amount, compound retention time and so on.
ChemStation Plus Security Pack—Graphical Result Review and Result Calculation Summary of version management in the ChemStation Plus Security Pack Each time a new result is calculated in the ChemStation, the application compares the values with the result values of the last reprocessed result copy. If it detects a difference, it automatically initializes the data storage in the database. Each data transfer of new results creates a new version entry in the database so that no data is ever overwritten.
ChemStation Plus Security Pack—Electronic Signatures and Password Security 21 CFR Part 11 permits the use of electronic signatures if the application ensures data integrity, data security and full audit-trail documentation. If an electronic signature is supposed to be equivalent to a handwritten signature it must contain at least two distinct identification components such as an identification code and a password.
ChemStation Plus Security Pack — Audit-trails and change documentation The Agilent ChemStation Plus Security Pack includes four audittrails: • run logbooks, • method revision history data, • sample audit-trail, and • database logbook. • all user comments during reanalysis cycles, and • a detailed change documentation of manual integration events. All reanalysis events and result versions are documented in the sample audit-trail.
manual interactive changes are: • change of custom field values • manual reintegration during reanalysis, • approval, rejection and retransfer to batch, • reloading data to disk, • archiving and dearchiving, and • re-opening of read-only runs.
ChemStation Plus Security Pack—Product Options and Configuration Standalone version The standalone version provides the ChemStation CD-ROM revision A.09.03 or higher and the ChemStation Plus CD-ROM revision B.02.02 or higher as described below. Description Product No. ChemStation Plus Security Pack. Adds the secure ChemStore C/S relational database add-on software module to the ChemStation Plus SW for A/D, GC, CE, LC and CE/LC-MSD. Supports 21 CFR Part 11.
4. Agilent ChemStation Plus Method Validation Pack Introduction A comprehensive understanding of the functionality of Agilent ChemStation Plus Method Validation Pack requires a brief introduction to the general aspects of method validation. The goal of method validation is “to provide documented evidence that a specific process will consistently provide results meeting the predetermined specifications.” This definition is taken from one of the FDA's method validation guidance documents.
Product description Agilent ChemStation Plus Method Validation Pack is a data management system for all method validation data. It includes advanced statistical calculations and result management in a relational database. Method Validation Pack offers a compound-centric design. For each compound it allows to define a set of tests (checkpoints) according to ICH, Pharmacopoeia or DIN guidelines.
Test execution Having completed the validation configuration, the experiments can be executed on an Agilent ChemStation Plus system. Method validation pack transfers the theoretical validation planning into a list of analytical runs by creating one or multiple ChemStation method validation sequences (MVS).
Result data entry and statistical calculations Data management and audittrails After completion of the analytical experiments the results can be uploaded from the ChemStore database into Method Validation Pack. The upload from ChemStore is an active and automated direct database data access. The transfer is executed as defined in the planning of the validation experiments. The analytical results are contained in the ChemStore database whereas the validation results are contained in Method Validation Pack.
ChemStation Plus Method Validation—System Requirements Compatibility with ChemStation Plus modules Agilent ChemStation Plus Method Validation Pack A.01.
Hard disk space Database size for Client-Server installation using Oracle database Standalone installation using Microsoft Access database Method Validation Pack needs approximately 40 MB hard disk space for installation. The validation files typically need 250–1000 KB per file. This depends on the size of embedded graphics. If possible, use vector graphics (WMFformat) rather than bitmap graphics (BMP) to reduce validation file size.
Working with ChemStation Plus Method Validation Pack General software operation Compatibility with Microsoft functionality Method Validation Pack is a Microsoft Windows program and can be operated via mouse clicks and keyboard in accordance with the Microsoft Windows standard. Users of Microsoft Windows programs should easily become familiar with operating Method Validation Pack.
All tasks are managed within the From planning to execution ChemStation Plus system. All 3)Experiment setup and data ChemStation Plus modules support management configuration data security, data integrity and (Level 3) audit-trails for comprehensive supa) Creation or update of port of FDA's requirements of elecChemStore study for all Method tronic records and electronic signaValidation Pack analytical tures.
User levels Top-level (Level 4 and 5): Validation setup and configuration Setup Method Validation Pack organizes data in method validation databases. A method validation database is the top-level container for all data that relate to one validation. All settings are linked to one validation database. For new validation files the software offers a master validation template that allows building new validations on the template.
others. Default entries for these headers can be defined when selecting the default header data button in the validation properties. Figure 25a shows table headers and default header data. Table Figure 25a Default header (grey) and header data header can only be changed or overwritten by changing the complete validation configuration while the default header data can be overwritten for every checkpoint.
• Robustness • Lab capability ( mainly used in non-pharmaceutical applications) • Calibration function • Limit of detection/quantification • Accuracy • Selectivity • Ring experiment (used to compare results among multiple laboratories) • Linearity The checkpoint configuration will typically depend on the compound type, and hardly any component requires execution of all checkpoints. The system therefore requires running the checkpoint configuration for each component individually.
Level 2: Data input After checkpoint configuration and planning is completed, users can now start data entry. This is the first result related step. Method Validation Pack offers three types of data input: 1. Automated data upload from the ChemStore database. Users select to load study data from the ChemStore method validation study and all data are automatically imported as configured in the Method Validation Pack Planning and described in the previous section 2.
ChemStation Method Validation Pack — Checkpoint Planning This section lists all checkpoints with their planning options and a short explanation of their meaning. Precision Precision describes the extent of conformity between results obtained during repeated use of a set analytical method under recurrent and comparable conditions. Monitoring the precision records random errors. Precision can be planned as precision in the true sense, or as repeatability from linearity.
• variance homogenity according to Bartlett. Lab capability Knowledge of lab capability is necessary for accurate estimates of process capability (see DIN 55350 parts 33 and 11). It checks for the ratio of result dispersion versus specifications. Lab capability occupies a special position among Validation concepts because it does not exclusively refer to the analytical method.
Linearity Linearity calculates a linear regression using the least square error for the model y = a + bx. Linearity can be carried out by multiple injections and multiple determinations. Figure 30 shows the planning dialog of checkpoint “linearity”.
Output settings for calculations • Vector y=ax+b - curve equation in the case of linearity • Square sum of the residuals (only calibration function) • Residual standard deviation • Mean value and standard deviation of y • Multiple correlation coefficient • Results of F- and t-tests • Method standard deviation Limit of detection and quantification The detection limit is the smallest amount of substance that can be detected qualitatively during one analysis with a defined statistical certainty.
Accuracy Accuracy describes the extent of correspondence between the expected value and the conventional value. Accuracy is influenced by the systematic error. The systematic error is divided into a constant systematic error and a proportional systematic error. A constant systematic error is not influenced by the concentration of the substance to be determined. If the error is influenced by the concentration, it is a proportional systematic error.
Planning data • Number of values • Y-units • Nominal value resolution R • Add chromatogram bitmap • Multiple injections possible Output settings All data are displayed Ring experiment Ring experiments are used to prove that a method can be transported to an entirely different location (other site, company etc.) and that it delivers good results. A ring experiment can be seen as a more general robustness. Figure 35 shows the planning dialog of the checkpoint “Ring experiment”.
ChemStation Plus Method Validation Pack — Interaction with other ChemStation Plus modules and ChemStore database As described in previous sections Method Validation Pack interacts with ChemStation for data acquisition and ChemStore for result and data management. Interaction with ChemStation for data acquisition If Method Validation Pack is installed in a ChemStation Plus data system ChemStation will offer additional functionality to run and execute method validation sequences.
Agilent ChemStation Plus Method Validation Pack — Interaction with ChemStore database tor only fills in the vial position for the samples and starts the sequence. For further details on ChemStation functionality, please refer to ChemStation specifications, Agilent Technologies publication number 5988-5314EN. ChemStore manages the analytical results along with the raw and meta data of the samples in a relational database.
ChemStation Plus Method Validation Pack — User Management and Access Rights Based on the hierarchical structure of the Method Validation Pack software, the system has five user levels. They are: 1) Reporting: Logging into the system with a name and a pass word of level 1 (reporting) gives you access to report output only. At this level, data changes are impossible.
Agilent ChemStation Plus Method Validation Pack — Data Security User authorization As mentioned under “User management”, only users with a valid ChemStation Plus user ID and their actual password can logon to the Method Validation Pack software. The user management includes a password policy for regular password renewal and user lockout after unsuccessful password entries. For details, please refer to ChemStation Plus Security Pack specifications.
tion (VDB-file), or clicking on its selection field, will restore the selected version. Documents and MVS files are displayed in a preview window, allowing to zoom, print, export or copy the selected document. The actions depend on the type of entry: documents are displayed in a preview window, validations are stored in the file system. DMS with standalone systems Standalone systems will typically require managing multiple databases.
Audit-trails Method Validation Pack audit-trail tracks all actions that users execute during program operation. The audit-trail is user-independent, can not be modified and it is completely system generated. Method Validation Pack has three different audit-trail levels, as shown in figure 41: • program audit-trail, • default validation audit-trail, and • validation audit-trail. The default display size of the audit-trail can be configured in the audit-trail window.
Default validation audit-trail The default validation audit-trail refers to the general configuration of validations. It covers all changes that are not related to a specific validation database but apply to all new and existing validations upon creation. These settings are new validation properties and new validation output settings. Changes to these settings are displayed in the default validation audit-trail. Validation audit-trail The Validation audit-trail tracks all actions on the actual validation.
Validation locking and electronic signatures After completion of a checkpoint, an entire component or a full validation, the validation can be locked partially or completely. To avoid locking of incomplete items, the application software will display a warning message and close the lock dialog without changes if the locking item is not complete. Partial validation locking allows locking a single checkpoint or a complete component. After locking the item, no changes are possible to this particular item.
Agilent ChemStation Plus Method Validation Pack — Installation Prerequisites Method Validation Pack can operate both PC-based in a standalone installation or in a networked system installation with full clientserver functionality. In both scenarios, some prerequisites must be met: Software ChemStation Plus standalone – For a fully integrated installation of Method Validation Pack it is required to have the following software installed: • ChemStore standalone rev. B.02.02 or higher or Security Pack rev. B.
ChemStation Plus Method Validation Pack — Product Options and Configurations Standalone version Description Product No. The standalone version of Method Validation Pack requires the additional installation of the ChemStation Plus database module for data management of analytical data. The database can be ordered as G2181BA ChemStore database or as G2183AA Security Pack for full support of 21 CFR Part 11. The installation only requires one of these products.
Installation, Qualification Services and Training Installation and familiarization Training Agilent Technologies’ installation and familiarization service ensure that the Agilent ChemStation Plus is installed correctly and in the right environment. Agilent’s ISO-registered trainings can save you time, help keep your laboratory operating costs low, broaden your capabilities, and ensure that your laboratory complies fully with regulatory and quality requirements.
