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Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS) 液相色谱法/串联质谱法(LC/MS/MS)测定水中溴敌隆、溴二氟康、敌鼠酮和华法林的标准试验方法
发布日期: 2023-04-15
1.1 本试验方法包括采用液相色谱法(LC)直接注射法和串联质谱法(MS/MS)检测法测定水中溴敌隆、溴鼠康、敌鼠酮和华法林(在本试验方法中统称为灭鼠剂)的含量。这些分析物通过该试验方法进行定性和定量测定。该测试方法遵循多重反应监测(MRM)质谱法。 1.2 灭鼠剂的检测验证等级(DVL)和报告范围列于 表1 。 1.2.1、 DVL的浓度要求至少比报告限值(RL)低3倍,且信噪比大于3:1。 图1 显示主要单反应监测(SRM)转换的信噪比,以及 图2 显示了杀鼠剂DVL处的确认SRM转变。 1.2.2 报告限值根据1级校准标准的浓度计算,如表4所示,考虑到用甲醇将40 mL水样稀释至50 mL的最终体积,以确保分析物的溶解度。 1.3 单位- 以国际单位制表示的数值应视为标准。本标准中不包括其他计量单位。 1.4 本标准并非旨在解决与其使用相关的所有安全问题(如有)。本标准的使用者有责任在使用前制定适当的安全、健康和环境实践,并确定监管限制的适用性。 1.5 本国际标准是根据世界贸易组织技术性贸易壁垒委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认的标准化原则制定的。 ====意义和用途====== 5.1 该测试方法由美国环保局芝加哥地区实验室(CRL)开发。 5.2 溴敌隆、溴大鼠、敌鼠酮和华法林是用于控制对公众健康、关键栖息地、本地动植物、作物、食物和水供应构成威胁的小鼠、大鼠和其他啮齿动物的灭鼠剂。这些灭鼠剂也带来了人类和环境安全问题。 华法林和敌鼠酮是第一代抗凝剂,溴敌隆和溴二氟康是第二代抗凝剂。抗凝血剂会干扰血液凝固,过量出血可能导致死亡。第二代抗凝剂特别危险,原因有几个。它们具有很高的毒性,并在身体组织中持续很长时间。第二代抗凝血剂被设计为在单次喂食中有毒,但死亡时间会在几天内发生。这使得啮齿动物在死亡前可以多次进食,导致尸体中含有的残留物可能是致命剂量的许多倍。 4. 5.3 该试验方法已被研究用于选定灭鼠剂的试剂、表面和饮用水。
1.1 This test method 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. ====== Significance And Use ====== 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.
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归口单位: D19.06
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