离子液体分散液相微萃取-HPLC检测血浆中溴敌隆

Determination of Bromadiolone in Plasma by Ionic Liquid Dispersive Liquid-liquid Microextraction and High Performance Liquid Chromatography

目的建立离子液体分散液相微萃取-HPLC检测血浆中溴敌隆的方法。方法以1-己基-3-甲基咪唑六氟磷酸盐([HMIM]PF6)为萃取剂,甲醇为分散剂,提取血浆中的溴敌隆,用HPLC分析其含量;考察了萃取剂和分散剂体积、样品pH值、NaCl浓度、萃取时间和离心时间等因素对萃取效率的影响。结果优化的溴敌隆分散液相微萃取操作条件为:萃取剂[HMIM]PF650μL,分散剂甲醇100μL,样品pH值5.0,萃取时间5min,离心时间8 min。方法的线性范围:0.01～5.0μg/mL,检测限:1.1 ng/mL(S/N>3)。该法低、中、高浓度的平均加标回收率分别为76.4%,82.6%,92.1%,RSD分别为4.17%,2.99%,1.67%(n=6)。结论本方法检测血浆中的溴敌隆,简便快速、准确实用,满足中毒检测及临床诊断治疗的需要。

Objective To develop a method for the determination of bromadiolone in plasma by ionic liquid dispersive liquid-liquid microextraction（DLLME） combined with high performance liquid chromatography（HPLC）.Methods 1-Hexyl-3-methylimidazoliumhexafluorophosphate（PF6） was used as extraction solvent and methanol was used as dispersant,bromadiolone in plasma was extracted and then was determined by HPLC.Some experimental parameters affecting the extraction efficiency,such as the volume of extraction solvent and dispersant,sample pH,salt concentration,extraction time and centrifuging time were investigated.Results The optimized extraction conditions were as follows： extraction solvent,PF6,50 μL;dispersant,methanol,100 μL;sample pH,5.0;extraction time,5 min;centrifuging time,8 min.Under the optimal extraction conditions,the linearity was obtained in the range of 0.01 ~ 5.0 μg/mL and the detection limit was 1.1ng/mL（S/N3）.This method provided acceptable recoveries（76.4 % ~ 92.1 %） and precisions（1.67 % ~ 4.17 %）.Conclusion This method is simple,rapid,accurate and practical for the determination of bromadiolone in plasma.