ASTM D7644-2016 采用液相色谱法/串联质谱法 (LC/MS/MS) 测定水中溴敌隆, 溴鼠灵, 敌鼠和杀鼠灵的标准试验方法
5.1x00a0;This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL). 5.2x00a0;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 5.3x00a0;This test method has been investigated for use with reagent, surface, and drinking water for the selected rodenticides. 1.1x00a0;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. 1.2x00a0;The Detection Verification Level (DVL) and Reporting Range for the rodenticides are listed in Table 1. 1.2.1x00a0;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. 1.2.2x00a0;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. 1.3x00a0;Unitsx2014;The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.4x00a0;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.
Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
(EU) No 703-2014 修订(EC) No 396/2005号法规的附录II、III和V中苯并噻二唑、乙氧喹啉、氟哇唑、异恶唑草酮、禾草敌、丙苯磺隆、吡草醚、灭藻醌、杀鼠灵在某些产品中的最大残留限量
ASTM D7644-2010e1 用液体色谱法/串联质谱法(LC/MS/MS)测定水中的三溴乙醇,塔隆,敌鼠,杀鼠灵的标准试验方法
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.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 Units8212;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.
Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
ASTM D7644-2010e2 用液相色谱法/串联质谱检测法(LC/MS/MS)测定水中溴敌隆,溴鼠灵,敌鼠和杀鼠灵的标准试验方法
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.1.1 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 Units8212;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 AnalyteDVL (ng/L)Reporting Range (ng/L) Bromadiolone20125-2500 Brodifacoum20125-2500 Diphacinone20125-2500 Warfarin20125-2500 FIG. 1 Example Primary SRM Chromatog......
Standard Test Method for Determination of Bromadiolone, Brodifacoum, Diphacinone and Warfarin in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
2006/5/EC-2006 欧盟委员会对将杀鼠灵归为活性物质的理事会指令91/414/EEC进行修订的指令
COMMISSION DIRECTIVE amending Council Directive 91/414/EEC to include warfarin as active substance
DB13/ 377-1998 杀鼠灵原药
本标准根据HG/丁2467.1-1996《农药原药产品标准编写规范》结合本省产 品特点制订。 本标准由河北省化学工业厅提出。 本标准由张家口双环国宝制药有限公司起草。 本标准主要起草人:王世河、李胜旺、王雪明、佟建华、史学忠。木标准规定了杀鼠灵原药的技术要求、试验方法、检验规则、标志、包装、运输和贮存。 本标准适用于由杀鼠灵及其生产中产生的杂质组成的杀鼠灵原药。
DOD A-A-53727 A-1993 美国标准杀鼠灵钠药片
The following National Stock Numbers are covered by this document
WARFARIN SODIUM TABLETS, USP
NC 29-12-1987 杀虫剂．杀鼠灵含量的光度剂测定
Esta norma establece el método de ensavo para la determina-ción fotométrica del contenido de warfarina en formulados y cebos.
Pesticides. Photometric Determinatíon of Warfarin Content
编辑：北检院编辑部
