ASTM D7644-16
Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

Standard No.

ASTM D7644-16

Release Date

2016

Published By

American Society for Testing and Materials (ASTM)

Status

Be replaced

Replace By

ASTM D7644-23

Latest

ASTM D7644-23

Scope

5.1 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).

5.2 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.4

5.3 This test method has been investigated for use with reagent, surface, and drinking water for the selected rodenticides.

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 test method. This test 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.

ASTM D7644-16 Referenced Document

• ASTM D1129 Standard Terminology Relating to Water
• ASTM D1193 Standard Specification for Reagent Water
• ASTM D2777 Standard Practice for Determination of Precision and Bias of Applicable Methods of Committee D-19 on Water
• ASTM D3694 Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
• ASTM D3856 Standard Guide for Good Laboratory Practices in Laboratories Engaged in Sampling and Analysis of Water
• ASTM D4841 Standard Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic Constituents
• ASTM D5847 Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
• ASTM E2554 Standard Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques

ASTM D7644-16 history

• 2023 ASTM D7644-23 Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
• 2016 ASTM D7644-16 Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
• 2010 ASTM D7644-10e2 Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
• 2010 ASTM D7644-10e1 Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
• 2010 ASTM D7644-10 Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)