ASTM E2549-2009 Standard Practice for Validation of Seized-Drug Analytical Methods《检获毒品分析方法的验证的标准实施规程》.pdf

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1、Designation: E 2549 09Standard Practice forValidation of Seized-Drug Analytical Methods1This standard is issued under the fixed designation E 2549; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number

2、 in 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 analytica

3、l 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 standard does not purport to address all of thesafety concerns, if any, associated with its use. It is therespo

4、nsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Significance and Use2.1 Validation is the confirmation by examination and theprovision of objective evidence that the particular req

5、uirementsfor 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 standard makes recommendations for the validation ofboth qualitative and quantitative methods

6、 used for the analysisof seized drugs.3. Analytical Scheme3.1 An analytical scheme shall be comprised of validatedmethods that are appropriate for the analyte.3.2 The combinations of methods chosen for a particularanalytical scheme shall identify the specific drug of interest,preclude a false positi

7、ve and minimize false negatives.3.3 For quantification the method should reliably determinethe amount of analyte present.3.4 If validated methods are used from published literatureor another laboratorys protocols, then the methods shall beverified within each laboratory3.5 If non-routine validated m

8、ethods are used, then themethod shall be verified prior to use.3.6 Verification should, at a minimum, demonstrate that arepresentative set of reference materials has been carriedthrough the process and yielded the expected results.4. Individual Laboratory Responsibility4.1 Each laboratory should det

9、ermine whether their currentstandard operating procedures have been validated, verified orrequire further validation/verification.5. Operational Environment5.1 All methods shall be validated or verified to demonstratethat they will perform in the normal operational environmentwhen used by individual

10、s expected to utilize the methods oncasework.6. Documentation6.1 The entire validation/verification process shall be docu-mented and the documentation shall be retained. Documenta-tion shall include, but is not limited to the following:6.1.1 personnel involved,6.1.2 dates,6.1.3 observations from the

11、 process,6.1.4 analytical data,6.1.5 a statement of conclusions and/or recommendations,and6.1.6 authorization approval signature.7. Recommendation7.1 To meet the requirements of sections 4 through 6,itisrecommended that laboratories follow the applicable provi-sions of Section 8 General Validation P

12、lan when validatingseized-drug analytical methods.NOTE 1For further information, see Supplemental Documents SD-2“Preparing Validation Plans, Section I: Analytical Techniques Elementsto Consider” and Section II: “Example Validation Plan for GC/MSIdentification and Quantitation of Heroin,” SWGDRUG.8.

13、General Validation Plan8.1 Purpose/ScopeThis is an introductory statement thatwill specify what is being tested, the purpose of the testing andthe result(s) required for acceptance.1This practice is under the jurisdiction of ASTM Committee E30 on ForensicSciences and is the direct responsibility of

14、Subcommittee E30.01 on Criminalistics.Current edition approved April 1, 2009. Published June 2009.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8.1.1 Performance SpecificationA list of specific objec-tives (e.g., trueness and preci

15、sion) should be determined priorto the validation process.8.1.2 Process Review After completion of the validationprocess the objectives should be revisited to ensure that theyhave been satisfactorily met.8.2 Analytical Method State exactly the method to bevalidated. It is essential that each step in

16、 the method bedemonstrated to perform satisfactorily. Steps that constitute amethod for the identification and/or quantification of seizeddrugs may include: visual characterization (e.g., macroscopic examination) determination of quantity of sample, which may include: weight volume item count sampli

17、ng (representative or random, dry, homogenized,etc.) stability of analyte sample preparation extraction method dissolution derivatization crystallization techniques for introducing sample into instrumentation instrumental parameters and specifications list the instruments and equipment (e.g., balanc

18、e andglassware) utilized instrument conditions software applications (e.g., software version, macros) calculations equation(s) to be used unit specification number of measurements required reference values significant figure conventions conditions for data rejection uncertainty determination.8.3 Ref

19、erence MaterialsAppropriate reference material(s)shall be used for qualitative and quantitative procedures.Traceability of the reference material is required.8.4 Performance Characteristics:8.4.1 SelectivityAssess the capability of the method toidentify/quantify the analyte(s) of interest, whether p

20、ure or in amixture.8.4.2 Matrix EffectsAssess the impact of any interferingcomponents and demonstrate that the method works in thepresence of substances that are commonly encountered inseized drug samples (e.g. cutting agents, impurities, by-products, precursors).8.4.3 RecoveryMay be determined for

21、quantitative analy-sis.8.4.4 Accuracy:8.4.4.1 Precision (Repeatability/Reproducibility)Determine the repeatability and reproducibility of all routinemethods. Conditions under which these determinations aremade shall be specified.NOTE 2Reproducibility determination may be limited to studieswithin the

22、 same laboratory.8.4.4.1.1 Within the scope of the validation, determineacceptable limits for repeatability and reproducibility.8.4.4.1.2 For qualitative analysis run the qualitative methoda minimum of ten times.8.4.4.1.3 For quantitative analysis run the quantitativemethod a minimum of ten times.8.

23、4.4.1.4 Validation criteria for non-routine methods maydiffer from what is stated above.8.4.4.2 Trueness:8.4.4.2.1 Trueness shall be determined for quantitativemethods to assess systematic error. Trueness can be assessedthrough various methods such as: comparison of a method-generated value for the

24、referencematerial with its known value using replicate measurements atdifferent concentrations performance of a standard addition method comparison to proficiency test results comparison with a different validated analytical method.8.4.5 RangeDetermine the concentration or sampleamount limits for wh

25、ich the method is applicable.8.4.5.1 Limit of Detection (LOD) Limit of detection shallbe determined for all qualitative methods.8.4.5.1.1 Determine the lowest amount of analyte that willbe detected and can be identified.8.4.5.1.2 The results obtained at the LOD are not necessar-ily quantitatively ac

26、curate.8.4.5.2 Limit of Quantitation (LOQ) Limit of Quantita-tion shall be determined for all quantitative methods. Deter-mine the lowest concentration that has an acceptable level ofuncertainty.8.4.5.3 Linearity Linearity shall be determined for allquantitative methods.8.4.5.3.1 Determine the mathe

27、matical relationship (calibra-tion curve) that exists between concentration and response overa selected range of concentrations.8.4.5.3.2 The LOQ effectively forms the lower end of theworking range.8.4.5.3.3 Determine the level of acceptable variation fromthe calibration curve at various concentrati

28、ons.8.4.5.3.4 Determine the upper limits of the working range.8.4.6 Robustness Robustness shall be determined foreither qualitative or quantitative methods. Alter method param-eters individually and determine any changes to accuracy.8.4.7 Ruggedness Ruggedness may be determined foreither qualitative

29、 or quantitative methods. Ruggedness shouldassess the factors external to the method.8.4.8 UncertaintyThe contribution of random and sys-tematic errors to method result uncertainty shall be assessedand the expanded uncertainty derived for quantitative methods.9. Quality Control9.1 Acceptance criteri

30、a for quality control parametersshould be adopted prior to implementation of the method.E2549092ASTM 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 determin

31、ation of the validity of any such patent rights, and 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 wit

32、hdrawn. Your comments are invited either for revision 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 yo

33、ur comments have not received a fair hearing you shouldmake 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).E2549093