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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2.2~18.5μg/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。
A post-column derivatization fluorescence detection high performance liquid chromatographic method was established for the determination of five kinds of coumarin rodenticide residues in the soil, such as warfarin, warfarin, bromadiolone, flufenoxamine and bromodextrin. The sample was extracted with a mixture of acetone-ammonia-methanol (100: 3: 100 by volume) after the internal standard chlorpromazine was added. The concentrated extract was extracted with 5 mL of n-hexane- The mixture was dissolved and NH2 SPE cartridge was purified. The analyte was eluted with 15 mL of 50 mmol / L tetrabutylammonium dihydrogen phosphate in methanol. The solvent was removed and the residue was washed with methanol-0.25% (volume fraction) aqueous acetic acid Ratio of 3: 2) was dissolved, filtered, separated by high performance liquid chromatography with methanol - ammonia - water (volume ratio of 1: 1: 8) mixture derived derivative reagent post column derivatization using a fluorescence detector Detection. The linear relationships of 5 warfarin, warfarin, bromadiolone, fluoxetine and bromodextrine in the range of 0.02-10.00 mg / L were good with the correlation coefficients above 0.999. The limits of quantification (LOQ, S / N = 10) was 2.2 to 18.5 μg / L. The recoveries of five rodenticides ranged from 94.6% to 118.0% and the relative standard deviations (RSDs) ranged from 0.8% to 10.2% (n = 3) at the 0.1-0.3 mg / kg level. Experimental results show that the method is sensitive, accurate and reproducible.