ASTM E2549-2014 Standard Practice for Validation of Seized-Drug Analytical Methods《确认扣押毒品分析方法的标准实施规程》.pdf

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1、Designation: E2549 14Standard Practice forValidation of Seized-Drug Analytical Methods1This standard is issued under the fixed designation E2549; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number i

2、n parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice addresses the validation of qualitative andquantitative seized-drug analytical methods. It discusses thevalidation of analytical

3、methods in terms of their part inanalytical schemes and in terms of performance characteristicsincluding brief mention of measurement uncertainty and qual-ity control parameters.1.2 This practice does not replace knowledge, skill, ability,experience, education or training and should be used inconjun

4、ction with professional judgment.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitat

5、ions prior to use.2. Referenced Documents2.1 ASTM Standards:2E2327 Practice for Quality Assurance of Laboratories Per-forming Seized-Drug AnalysisE2764 Practice for UncertaintyAssessment in the Context ofSeized-Drug Analysis3. Significance and Use3.1 Validation is the confirmation by examination and

6、 theprovision of objective evidence that the particular requirementsfor a specific intended use are fulfilled. There are numerousdocuments that address the topic of validation but there are fewvalidation protocols for methods specific to seized drug analy-sis. This practice makes recommendations for

7、 the validation ofboth qualitative and quantitative methods used for the analysisof seized drugs.4. Analytical Scheme4.1 An analytical scheme shall be comprised of validatedmethods that are appropriate for the analyte.4.2 The combinations of methods chosen for a particularanalytical scheme shall ide

8、ntify the specific drug of interest,preclude a false positive and minimize false negatives.4.3 For quantification the method should reliably determinethe amount of analyte present.4.4 If validated methods are used from published literatureor another laboratorys protocols, then the methods shall beve

9、rified within each laboratory4.5 If non-routine validated methods are used, then themethod shall be verified prior to use.4.6 Verification should, at a minimum, demonstrate that arepresentative set of reference materials has been carriedthrough the process and yielded the expected results.5. Individ

10、ual Laboratory Responsibility5.1 Each laboratory should determine whether their currentstandard operating procedures have been validated, verified, orrequire further validation/verification.6. Operational Environment6.1 All methods shall be validated or verified to demonstratethat they will perform

11、in the normal operational environmentwhen used by individuals expected to utilize the methods oncasework.7. Documentation7.1 The entire validation/verification process shall be docu-mented and the documentation shall be retained for a period inaccordance with laboratory policy. Documentation shallin

12、clude, but is not limited to the following:7.1.1 Personnel involved;7.1.2 Dates;7.1.3 Observations from the process;7.1.4 Analytical data;7.1.5 A statement of conclusions or recommendations, orboth; and7.1.6 Authorization approval signature.1This practice is under the jurisdiction of ASTM Committee

13、E30 on ForensicSciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.Current edition approved March 1, 2014. Published March 2014. Originallyapproved in 2009. Last previous edition approved in 2009 as E2549 09. DOI:10.1520/E2549-14.2For referenced ASTM standards, visit t

14、he ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959.

15、United States18. Recommendation8.1 To meet the requirements of Sections 4 through 7,itisrecommended that laboratories follow the applicable provi-sions of Section 9 General Validation Plan when validatingseized-drug analytical methods.NOTE 1For further information, see http:/www.swgdrug.org forSuppl

16、emental Documents SD-2 “Preparing Validation Plans, Section I:Analytical Techniques Elements to Consider” and Section II: “ExampleValidation Plan for GC/MS Identification and Quantitation of Heroin,”SWGDRUG.9. General Validation Plan9.1 Purpose/ScopeThis is an introductory statement thatwill specify

17、 what is being tested, the purpose of the testing andthe result(s) required for acceptance.9.1.1 Performance SpecificationA list of specific objec-tives (for example, trueness and precision) should be deter-mined prior to the validation process.9.1.2 Process ReviewAfter completion of the validationp

18、rocess the objectives should be revisited to ensure that theyhave been satisfactorily met.9.2 Analytical MethodState exactly the method to bevalidated. It is essential that each step in the method bedemonstrated to perform satisfactorily. Steps that constitute amethod for the identification or quant

19、ification, or both, ofseized drugs may include:Visual characterization (for example, macroscopic examination)Determination of quantity of sample, which may include:WeightVolumeItem countSampling (representative or random, dry, homogenized, etc.)Stability of analyteSample preparation:Extraction metho

20、dDissolutionDerivatizationCrystallizationTechniques for introducing sample into instrumentationInstrumental parameters and specifications:List the instruments and equipment (for example, balance andglassware) utilizedInstrument conditionsSoftware applications (for example, software version, macros)C

21、alculations:Equation(s) to be usedUnit specificationNumber of measurements requiredReference valuesSignificant figure conventionsConditions for data rejectionUncertainty determination9.3 Reference MaterialsAppropriate reference material(s)(see Practice E2327) shall be used to develop and validateana

22、lytical procedures for qualitative and quantitative proce-dures. The validation documentation and operating protocolshould define the frequency of usage of the relevant referencematerials and their minimum specification (for example, saltform, minimum purity, isomeric form). Traceability of therefer

23、ence material is required.9.4 Performance Characteristics:9.4.1 SelectivityAssess the capability of the method toidentify/quantify the analyte(s) of interest, whether pure or in amixture.9.4.2 Matrix EffectsAssess the impact of any interferingcomponents and demonstrate that the method works in thepr

24、esence of substances that are commonly encountered inseized drug samples (for example, cutting agents, impurities,by-products, precursors).9.4.3 RecoveryMay be determined for quantitative analy-sis.9.4.4 Accuracy:9.4.4.1 Precision (Repeatability/Reproducibility)Determine the repeatability and reprod

25、ucibility of all routinemethods. Conditions under which these determinations aremade shall be specified.NOTE 2Reproducibility determination may be limited to studieswithin the same laboratory.(1) Within the scope of the validation, determine accept-able limits for repeatability and reproducibility.(

26、2) For qualitative analysis, run the qualitative method aminimum of ten times.(3) For quantitative analysis, run the quantitative method aminimum of ten times.(4) Validation criteria for non-routine methods may differfrom what is stated above.9.4.4.2 Trueness:(1) Trueness shall be determined for qua

27、ntitative methodsto assess systematic error. Trueness can be assessed throughvarious methods such as: Comparison of a method-generated value for the refer-ence material with its known value using replicate measure-ments at different concentrations, Performance of a standard addition method, Comparis

28、on to proficiency test results, and Comparison with a different validated analytical method.9.4.5 RangeDetermine the concentration or sampleamount limits for which the method is applicable.9.4.5.1 Limit of Detection (LOD)Limit of detection shallbe determined for all qualitative methods.(1) Determine

29、 the lowest amount of analyte that will bedetected and can be identified.(2) The results obtained at the LOD are not necessarilyquantitatively accurate.9.4.5.2 Limit of Quantitation (LOQ)Limit of Quantitationshall be determined for all quantitative methods. Determine thelowest concentration that has

30、 an acceptable level of uncer-tainty.9.4.5.3 LinearityLinearity shall be determined for allquantitative methods.(1) Determine the mathematical relationship (calibrationcurve) that exists between concentration and response over aselected range of concentrations.(2) The LOQ effectively forms the lower

31、 end of theworking range.(3) Determine the level of acceptable variation from thecalibration curve at various concentrations.(4) Determine the upper limits of the working range.9.4.6 RobustnessRobustness shall be determined for ei-ther qualitative or quantitative methods. Alter method param-eters in

32、dividually and determine any changes to accuracy.E2549 1429.4.7 RuggednessRuggedness may be determined for ei-ther qualitative or quantitative methods. Ruggedness shouldassess the factors external to the method.9.4.8 UncertaintyThe contribution of random and system-atic errors to method result uncer

33、tainty shall be assessed andthe expanded uncertainty derived for quantitative methods (seePractice E2764).10. Quality Control10.1 Acceptance criteria for quality control parametersshould be adopted prior to implementation of the method.11. Keywords11.1 analytical scheme; methods; performance charact

34、eris-tics; seized-drug analytics; validationASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and

35、 the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revisio

36、n of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you sho

37、uldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).E2549 143