摘要：建立了测定土壤中杀鼠灵、杀鼠醚、溴敌隆、氟鼠灵、溴鼠隆5种香豆素类灭鼠药残留量的柱后衍生荧光检测高效液相色谱方法。样品在加入内标物氯杀鼠灵后用丙酮-氨水-甲醇（体积比为100：3：100）混合液提取，浓缩的提取液用5 mL正己烷-氯仿（体积比为3：1）混合液溶解，NH₂固相萃取小柱净化，用15 mL 50 mmol/L四丁基磷酸二氢铵甲醇溶液洗脱分析物，移除溶剂，用甲醇-0.25%（体积分数）乙酸水溶液（体积比为3：2）混合液溶解，过滤后，经高效液相色谱分离，以甲醇-氨水-水（体积比为1：1：8）混合液为衍生试剂进行柱后衍生，采用荧光检测器检测。杀鼠灵、杀鼠醚、溴敌隆、氟鼠灵、溴鼠隆5种鼠药在0.02～10.00 mg/L范围内线性关系良好，相关系数均大于0.999，定量限（LOQ，S/N=10）为2.2～18.5 μg/L。在0.1～0.3 mg/kg添加水平内，5种灭鼠药的回收率为94.6%～118.0%，相对标准偏差（RSD）为0.8%～10.2% （n=3）。实验结果表明该方法灵敏、准确，重复性好。

Abstract: A method for the determination of warfarin, coumatetralyl, bromadiolone, flocoumafen and brodifacoum residues in soils with post-column derivatization and fluorescence detection by high performance liquid chromatography (HPLC) was established. The samples were extracted with a mixed solution of acetone, ammonium and methanol (100:3:100, v/v/v) after adding ratilan as internal standard. The extracts were vacuum-concentrated and dissolved in 5 mL mixed solution of hexane and chloroform (3:1, v/v) for solid phase extraction (SPE) clean up on an aminopropyl column. The analytes were eluted from the column using 15 mL of 50 mmol/L tetrabutylammonium dihydrogen phosphate in methanol. The solvent was evaporated and the sample was dissolved in a mixed solution of methanol and 0.25% (v/v) acetic acid aqueous solution (3:2, v/v). The coumarin rodenticides were separated on a C₁₈ column by HPLC and on-line derivatized with a mixed solution of methanol, ammonium and water (1:1:8, v/v/v) and detected with a fluorescence detector. Good linearities of the analytes were achieved over the mass concentration of 0.02-10.00 mg/L, with correlation coefficients above 0. 999. The limits of quantification (LOQ, S/N=10) were 2.2-18.5 μg/L for the five coumarin rodenticides. The recoveries were 94.6%-118.0% at the spiked levels of 0.1-0.3 mg/kg in soil with the relative standard deviations of 0.8%-10.2% (n=3). The results indicated that the method is sensitive and accurate with repeatability.