Significance and Use

This test method has been developed by US EPA 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.

1. 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.

1.3 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.

TABLE 1 Detection Verification Level and Reporting Range

FIG. 1 Example Primary SRM Chromatograms Signal/Noise Ratios

FIG. 2 Example Confirmatory SRM Chromatograms Signal/Noise Ratios

2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

ASTM Standards

D1129 Terminology Relating to Water

D1193 Specification for Reagent Water

D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water

D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents

D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water

D4841 Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic Constituents

D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis

E2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method in a Single Laboratory Using a Control Sample Program

Other Documents

Keywords

liquid chromatography; mass spectrometry; rodenticides; water; Liquid chromatography (LC)--water analysis; Mass spectrometry--water; Rodenticides; Water analysis

ICS Code

ICS Number Code 13.060.50 (Examination of water for chemical substances)

DOI: 10.1520/D7644-10E02

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ASTM D7644