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.

1.2 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.

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/D7644-10

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