Hunter K
J Chromatogr. 1985 Mar 15;321(2):255-72. doi: 10.1016/s0021-9673(01)90444-3.
A comprehensive approach to the analysis of anticoagulant rodenticide residues in animal tissues based on high-performance liquid chromatography (HPLC) has been developed. Residues of warfarin, coumatetralyl, difenacoum, brodifacoum, bromadiolone, diphacinone and chlorophacinone were extracted with chloroformacetone (1:1, v/v). Extracts were cleaned-up by an integrated gel permeation and adsorption chromatographic procedure which divided the rodenticides into two groups. Residues were then determined and confirmed using normal-phase, ion-pair and weak ion-exchange HPLC techniques. Ion-pair gradient separation resolved all seven rodenticides in a single chromatographic analysis. UV detection methods were employed for all seven rodenticides. Use of a diode array detection system permitted additional confirmation of residues down to 0.1 mg kg-1 by matching UV spectra and derivatives of spectra. Sensitive fluorescence detection was possible for the coumarin-based rodenticides but not for diphacinone and chlorophacinone. Post-column pH-switching fluorescence detection methods were shown to be superior to other methods of fluorescence detection of coumarin-based rodenticides. Recoveries from spiked liver tissue were around 90% at levels from 0.05 to 1 mg kg-1. Detection limits of around 0.002 mg kg-1 for most rodenticides and of 0.01 mg kg-1 for warfarin could be achieved with animal tissue extracts.
已开发出一种基于高效液相色谱（HPLC）分析动物组织中抗凝血灭鼠剂残留的综合方法。用氯仿 - 丙酮（1:1，v/v）提取华法林、杀鼠迷、敌鼠隆、溴敌隆、溴鼠灵、敌鼠和氯敌鼠的残留。提取物通过集成凝胶渗透和吸附色谱程序进行净化，该程序将灭鼠剂分为两组。然后使用正相、离子对和弱离子交换HPLC技术测定并确证残留。离子对梯度分离在一次色谱分析中可分离出所有七种灭鼠剂。对所有七种灭鼠剂均采用紫外检测方法。使用二极管阵列检测系统，通过匹配紫外光谱和光谱衍生物，可进一步确证低至0.1 mg kg-1的残留。基于香豆素的灭鼠剂可进行灵敏的荧光检测，但敌鼠和氯敌鼠则不能。柱后pH转换荧光检测方法被证明优于基于香豆素的灭鼠剂的其他荧光检测方法。在加标肝组织中，0.05至1 mg kg-1水平的回收率约为90%。动物组织提取物对大多数灭鼠剂的检测限约为0.002 mg kg-1，对华法林的检测限为0.01 mg kg-1。
