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METHODS, METHOD VERIFICATION AND VALIDATION

METHODS, METHOD VERIFICATION AND VALIDATION

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Published by jljimenez1969
This document is uncontrolled when printed. For the current and official copy, check the Intranet at http://web.ora.fda.gov/dfs/policies/manuals/default.htm
This document is uncontrolled when printed. For the current and official copy, check the Intranet at http://web.ora.fda.gov/dfs/policies/manuals/default.htm

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Published by: jljimenez1969 on Aug 27, 2008
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06/11/2013

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Version No.: 1.2
ORA LABORATORY PROCEDUREFood and Drug Administration
Document No.:
ORA-LAB.5.4.5
 
Page 1 of 14Title:
METHODS, METHOD VERIFICATION AND VALIDATION
Effective Date:10-01-03Revised: 09-09-05
This document is uncontrolled when printed: 9/12/2005For the current and official copy, check the Intranet athttp://web.ora.fda.gov/dfs/policies/manuals/default.htm 
Sections Included in this Document and Document History
1. Purpose2. Scope3. Responsibilities4. Background5. References6. Procedure7. Definitions8. Records9. Supporting Documents10. Attachments11. AppendicesDocument History
 
1.Purpose
 
This document establishes the guidelines for method selection and theprocedures for verification of standard method performance, as well as thevalidation of non-standard methods.
2.Scope
 
ORA laboratories verify standard method performance and validate non-standard methods introduced into the laboratory.
3.Responsibilities
 
A.
 
Directors:
 
ensures implementation of method verification and validationprocedures.B.
 
Supervisors:
 
implements method verification and validation procedures in respectivedivision.C. Staff:
 
adheres to written protocol for method performance verification,validation or modification.
4.Background
 
None
5.References
 
 A Laboratory Guide to Method Validation
, (Eurachem).
 
Version No.: 1.2
ORA LABORATORY PROCEDUREFood and Drug Administration
Document No.:
ORA-LAB.5.4.5
 
Page 2 of 14Title:
METHODS, METHOD VERIFICATION AND VALIDATION
Effective Date:10-01-03Revised: 09-09-05
This document is uncontrolled when printed: 9/12/2005For the current and official copy, check the Intranet athttp://web.ora.fda.gov/dfs/policies/manuals/default.htm 
6.Procedure6.1 MethodSelection6.2StandardMethodVerification
6.3MethodValidation
A.
 
Selection of MethodsAn integral part of the laboratory quality system is the use of standardmethods. Standard methods are used, whenever possible, or unlessotherwise specified by the Compliance Program or the customer. Non-standard methods are used in cases where a standard method does not existand the customer has agreed to its use. A clear expression of qualityobjectives and testing parameters or criteria are made when a non-standard method is employed.A.
 
Standard or FDA
official
methods need verification to ensure that thelaboratory is capable of performing the analysis. The laboratory’s qualitycontrol program as described in ORA-LAB.5.9 addresses this need.Verification of an analytical procedure is the demonstration that alaboratory is capable of replicating with an acceptable level of performance a standard method. Verification under conditions of use isdemonstrated by meeting system suitability specifications established forthe method, as well as a demonstration of accuracy and precision or othermethod parameters for the type of method. Method performance isaccomplished by using performance characteristics such as:
 
blanks in chemistry, or un-inoculated media in microbiology, to assesscontamination;
 
laboratory control samples - spiked samples for chemistry or positiveculture controls for microbiology, to assess accuracy;
 
precision based on the analysis of duplicates;
 
calibration check standards analyzed periodically in the analyticalbatch for quantitative analyses; and
 
monitoring quality control samples, usually through the use of controlcharts.A.
 
Validation of Method Performance1.
 
Non-standard and laboratory-developed methods need methodvalidation. This activity is planned and assigned to qualified personnel.The method’s performance characteristics are based on the intended
 
Version No.: 1.2
ORA LABORATORY PROCEDUREFood and Drug Administration
Document No.:
ORA-LAB.5.4.5
 
Page 3 of 14Title:
METHODS, METHOD VERIFICATION AND VALIDATION
Effective Date:10-01-03Revised: 09-09-05
This document is uncontrolled when printed: 9/12/2005For the current and official copy, check the Intranet athttp://web.ora.fda.gov/dfs/policies/manuals/default.htm 
use of the method. For example, if the method will be used forqualitative analysis, there is no need to test and validate the method’slinearity over the full dynamic range of the equipment.2.
 
Typical validation characteristics which should be considered are:
 
accuracy,
 
precision,
 
specificity,
 
detection limit,
 
limit of quantitation,
 
linearity,
 
range, and
 
ruggedness and robustness.See Section 7 for definitions of these characteristics.B.
 
Validation ToolsThe following tools can be used to demonstrate the ability to meet methodspecifications of performance:1.
 
 Blanks:
Use of various types of blanks enables assessment of howmuch is attributable to the analyte and how much is attributable to othercauses.2.
 
 Reference materials and certified reference materials:
Use of knownmaterials can be used to assess the accuracy of the method, as well asobtaining information on interferences.3.
 
Fortified (spiked) materials and solutions:
Recovery determinationscan be made from fortification or spiking with a known amount of analyte.4.
 
 Incurred materials:
These are materials in which the analyte of interestmay be essentially alien, but has been introduced to the bulk at somepoint prior to the material being samples.5.
 
 Measurement standards:
These are substances used for calibration oridentification purposes. When placed periodically in an analyticalbatch, checks can be made that the response of the analytical process tothe analyte is stable.

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