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血清和肝脏中八种抗凝血灭鼠剂的同时测定

Simultaneous determination of eight anticoagulant rodenticides in blood serum and liver.

作者信息

Chalermchaikit T, Felice L J, Murphy M J

机构信息

Department of Veterinary Diagnostic Medicine, College of Veterinary Medicine, University of Minnesota, St. Paul 55108.

出版信息

J Anal Toxicol. 1993 Jan-Feb;17(1):56-61. doi: 10.1093/jat/17.1.56.

DOI:10.1093/jat/17.1.56
PMID:8429630
Abstract

A liquid chromatographic method was developed for the analysis of indandione and 4-hydroxycoumarin anticoagulant rodenticides in blood serum and liver. The method enabled the measurement of serum and liver concentrations of eight anticoagulant rodenticides: brodifacoum, bromadiolone, chlorophacinone, coumafuryl, coumatetralyl, diphacinone, difenacoum, and warfarin. Anticoagulants were extracted from serum and liver with acetonitrile. Extracts were applied to solid-phase extraction columns, which contained mixed packings. Column eluates were evaporated to dryness, reconstituted, and subjected to reversed-phase liquid chromatography. Hydroxycoumarins were detected by fluorescence at an excitation wavelength of 318 nm and an emission wavelength of 390 nm. Indandiones were detected by UV absorption at 285 nm. Extraction efficiencies of greater than 75% for serum and greater than 69% for liver were obtained. The within-run precision (CV) ranged from 2.4 to 8.6% for serum and 2.6 to 8.7% for liver. The between-run precision (CV) ranged from 1.5 to 12.2% for serum and from 2.1 to 11.8% for liver. Hydroxycoumarin rodenticides were detected at 1 ng/mL of serum and 1 ng/g of liver. Indandiones were detected at 10 ng/mL of serum and 10 ng/g of liver.

摘要

建立了一种液相色谱法,用于分析血清和肝脏中的茚满二酮和4-羟基香豆素类抗凝血灭鼠剂。该方法能够测定8种抗凝血灭鼠剂在血清和肝脏中的浓度,这些灭鼠剂包括:溴敌隆、溴鼠灵、氯鼠酮、杀鼠呋、杀鼠醚、敌鼠、二氟鼠酮和华法林。抗凝血剂用乙腈从血清和肝脏中提取。提取物应用于装有混合填料的固相萃取柱。柱洗脱液蒸发至干,复溶后进行反相液相色谱分析。羟基香豆素在激发波长318nm和发射波长390nm处通过荧光检测。茚满二酮在285nm处通过紫外吸收检测。血清的提取效率大于75%,肝脏的提取效率大于69%。批内精密度(CV)血清为2.4%至8.6%,肝脏为2.6%至8.7%。批间精密度(CV)血清为1.5%至12.2%,肝脏为2.1%至11.8%。羟基香豆素类灭鼠剂在血清浓度为1ng/mL和肝脏浓度为1ng/g时可被检测到。茚满二酮在血清浓度为10ng/mL和肝脏浓度为10ng/g时可被检测到。

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