ASTM D7644-10e1
(Test Method)Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
SIGNIFICANCE AND USE
This test method has been developed in support of the National Homeland Security Research Center, US EPA by Region 5 Chicago Regional Laboratory (CRL).
Bromadiolone, brodifacoum, diphacinone and warfarin are rodenticides for controlling mice, rats, and other rodents that pose a threat to public health, critical habitats, native plants and animals, crops, food and water supplies. These rodenticides also present human and environmental safety concerns. Warfarin and diphacinone are first-generation anticoagulants, while bromadiolone and brodifacoum are second-generation. The anticoagulants interfere with blood clotting, and death can result from excessive bleeding. The second-generation anticoagulants are especially hazardous for several reasons. They are highly toxic and persist a long time in body tissues. The second-generation anticoagulants are designed to be toxic in a single feeding, but time-to-death occurs in several days. This allows rodents to feed multiple times before death, leading to carcasses containing residues that may be many times the lethal dose.
This method has been investigated for use with reagent, surface, and drinking water for the selected rodenticides.
SCOPE
1.1 This procedure covers the determination of bromadiolone, brodifacoum, diphacinone and warfarin (referred to collectively as rodenticides in this test method) in water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry.
1.2 The Detection Verification Level (DVL) and Reporting Range for the rodenticides are listed in Table 1.
1.2.1 The DVL is required to be at a concentration at least 3 times below the Reporting Limit (RL) and have a signal/noise ratio greater than 3:1. Fig. 1 displays the signal/noise ratios of the primary single reaction monitoring (SRM) transitions, and Fig. 2 displays the confirmatory SRM transitions at the DVLs for the rodenticides.
1.2.2 The reporting limit was calculated from the concentration of the Level 1 calibration standard, as shown in Table 4, accounting for the dilution of a 40 mL water sample up to a final volume of 50 mL with methanol to ensure analyte solubility.
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
General Information
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Standards Content (Sample)
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Contact ASTM International (www.astm.org) for the latest information
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Designation: D7644 – 10
Standard Test Method for
Determination of Bromadiolone, Brodifacoum, Diphacinone
and Warfarin in Water by Liquid Chromatography/Tandem
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Mass Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D7644; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
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´ NOTE—Test Method was corrected editorially in 2011
TABLE 1 Detection Verification Level and Reporting Range
1. Scope
DVL Reporting Range
1.1 This procedure covers the determination of bromadi-
Analyte
(ng/L) (ng/L)
olone, brodifacoum, diphacinone and warfarin (referred to
Bromadiolone 20 125-2500
collectively as rodenticides in this test method) in water by
Brodifacoum 20 125-2500
directinjectionusingliquidchromatography(LC)anddetected
Diphacinone 20 125-2500
Warfarin 20 125-2500
with tandem mass spectrometry (MS/MS). These analytes are
qualitatively and quantitatively determined by this method.
This method adheres to multiple reaction monitoring (MRM)
2. Referenced Documents
mass spectrometry.
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1.2 The Detection Verification Level (DVL) and Reporting
2.1 ASTM Standards:
Range for the rodenticides are listed in Table 1.
D1129 Terminology Relating to Water
1.2.1 The DVL is required to be at a concentration at least
D1193 Specification for Reagent Water
3 times below the Reporting Limit (RL) and have a signal/
D2777 Practice for Determination of Precision and Bias of
noise ratio greater than 3:1. Fig. 1 displays the signal/noise
Applicable Test Methods of Committee D19 on Water
ratios of the primary single reaction monitoring (SRM) transi-
D3694 Practices for Preparation of Sample Containers and
tions, and Fig. 2 displays the confirmatory SRM transitions at
for Preservation of Organic Constituents
the DVLs for the rodenticides.
D3856 Guide for Good Laboratory Practices in Laborato-
1.2.2 The reporting limit was calculated from the concen-
ries Engaged in Sampling and Analysis of Water
tration of the Level 1 calibration standard, as shown inTable 4,
D4841 Practice for Estimation of Holding Time for Water
accounting for the dilution of a 40 mL water sample up to a
Samples Containing Organic and Inorganic Constituents
final volume of 50 mL with methanol to ensure analyte
D5847 Practice for Writing Quality Control Specifications
solubility.
for Standard Test Methods for Water Analysis
1.3 Units—The values stated in SI units are to be regarded
E2554 Practice for Estimating and Monitoring the Uncer-
as standard. No other units of measurement are included in this
tainty of Test Results of a Test Method in a Single
standard.
Laboratory Using a Control Sample Program
1.4 This standard does not purport to address all of the
2.2 Other Documents:
safety concerns, if any, associated with its use. It is the
EPApublication SW-846 Test Methods for Evaluating Solid
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responsibility of the user of this standard to establish appro-
Waste, Physical/Chemical Methods
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
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This test method is under the jurisdiction of ASTM Committee D19 on Water Standards volume information, refer to the standard’s Document Summary page on
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor the ASTM website.
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Organic Substances in Water. Available from National Technical Information Service (NTIS), U.S. Depart-
Current edition approved June 1, 2010. Published April 2011 Last previous ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
edition published in 2010 as D7644–10. DOI: 10.1520/D7644-10E01. www.epa.gov/epawaste/hazard/testmethods/index.htm.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D7644 – 10
FIG. 1 Example Primary SRM Chromatograms Signal/Noise Ratios
FIG. 2 Example Confirmatory SRM Chromatograms Signal/Noise Ratios
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D7644 – 10
3. Terminology allows rodents to feed multiple times before death, leading to
carcassescontainingresiduesthatmaybemanytimesthelethal
3.1 Definitions:
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dose.
3.1.1 detection verification level, DVL, n—a concentration
5.3 This method has been investigated for use with reagent,
thathasasignal/noise(S/N)ratiogreaterthan3:1andisatleast
surface, and drinking water for the selected rodenticides.
3 times below the Reporting Limit (RL
...
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