1、Designation:D7644102Standard Test Method forDetermination of Bromadiolone,Brodifacoum,Diphacinoneand Warfarin in Water by Liquid Chromatography/TandemMass Spectrometry(LC/MS/MS)1This standard is issued under the fixed designation D7644;the number immediately following the designation indicates the y
2、ear oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1NOTEThis test method was corrected editorially in April 2011.2NOTEThis
3、 test method was corrected editorially in February 2012.1.Scope1.1 Thisprocedurecoversthedeterminationofbromadiolone,brodifacoum,diphacinone and warfarin(re-ferred to collectively as rodenticides in this test method)inwater by direct injection using liquid chromatography(LC)anddetected with tandem m
4、ass spectrometry(MS/MS).Theseanalytes are qualitatively and quantitatively determined by thismethod.This method adheres to multiple reaction monitoring(MRM)mass spectrometry.1.2 The Detection Verification Level(DVL)and ReportingRange for the rodenticides are listed in Table 1.1.2.1 The DVL is requir
5、ed to be at a concentration at least3 times below the Reporting Limit(RL)and have a signal/noise ratio greater than 3:1.Fig.1 displays the signal/noiseratios of the primary single reaction monitoring(SRM)transitions,and Fig.2 displays the confirmatory SRM transi-tions at the DVLs for the rodenticide
6、s.1.2.2 The reporting limit was calculated from the concen-tration of the Level 1 calibration standard,as shown in Table 4,accounting for the dilution of a 40 mL water sample up to afinal volume of 50 mL with methanol to ensure analytesolubility.1.3 UnitsThe values stated in SI units are to be regar
7、dedas standard.No other units of measurement are included in thisstandard.1.4 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 th
8、e applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3694 Practices for Prep
9、aration of Sample Containers andfor Preservation of Organic ConstituentsD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD4841 Practice for Estimation of Holding Time for WaterSamples Containing Organic and Inorganic ConstituentsD5847 Practice for Writing Quality Control
10、 Specificationsfor Standard Test Methods for Water AnalysisE2554 Practice for Estimating and Monitoring the Uncer-tainty of Test Results of a Test Method Using ControlChart Techniques2.2 Other Documents:EPA publication SW-846 Test Methods for Evaluating SolidWaste,Physical/Chemical Methods33.Termino
11、logy3.1 Definitions:3.1.1 detection verification level,DVL,na concentrationthat has a signal/noise(S/N)ratio greater than 3:1 and is at least3 times below the Reporting Limit(RL).3.1.2 reporting limit,RL,nthe concentration of thelowest-level calibration standard used for quantification ac-counting f
12、or the sample dilution.3.1.2.1 DiscussionIn this test method,a 40 mL samplealiquot is diluted to a 50 mL final volume after thoroughly1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Su
13、bstances in Water.Current edition approved June 1,2010.Published February 2011.DOI:10.1520/D7644-10E02.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Docu
14、ment Summary page onthe ASTM website.3Available from National Technical Information Service(NTIS),U.S.Depart-ment of Commerce,5285 Port Royal Road,Springfield,VA,22161 or at http:/www.epa.gov/epawaste/hazard/testmethods/index.htm.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Co
15、nshohocken,PA 19428-2959.United States1 rinsing the collection vial with methanol for quantitativetransfer.In this case,the lowest calibration level of 100 pptwould allow a reporting limit of 125 ppt to be achieved.3.1.3 rodenticides,nin this test method,bromadiolone,brodifacoum,diphacinone,and warf
16、arin collectively.3.2 Abbreviations:3.2.1 mMmillimolar,1 10-3moles/L3.2.2 NDnon-detect3.2.3 pptparts per trillion,ng/L4.Summary of Test Method4.1 This is a performance based method,and modificationsare allowed to improve performance.4.2 For rodenticide analysis,samples are shipped to the labbetween 0C and 6C and analyzed within 14 days of collec-tion.In the lab,the samples are spiked with surrogates,quantitatively transferred to a graduated cylinder using threemethanol rinses,filtered using a sy
