首页> 中文期刊>中国法医学杂志 >应用分子印迹固相萃取法提取血液中大隆和溴敌隆

应用分子印迹固相萃取法提取血液中大隆和溴敌隆

     

摘要

Objecive Molecular imprinted polymer are used as solid-phase extraction agents to extract brodifacoum and bromoadiolone from blood samples. Methods The brodifacoum imprinted molecule is synthesized with the ratio of 1 mol brodifacoum template molecule to 4 mol acrylamide monomer molar. The solid-phase extraction ( SPE) procedure is suggested as; elute interferences are washed out with 1 mL DI water twice and 1 ml 30% MeOH once respectively; brodifacoum and bromoadiolone are eluted with 1 mL 1% formic acid in methanol twice. Concentrated elution is analyzed with UPLC-MS. Results The recoveries of brodifacoum and bromoadiolone are larger than 90%. A good linear relationship, correlation coefficients 0. 99, is obtained at the concentration range 50 ~500 ng/mL. The limit of detection is prior than 10 ng/mL for signal to noise ratio(S/N) being 5:1. Conclusion The proposed method is of high recovery rate, reduce matrix effects, less interference of impurities. It can be used to extract brodifacoum and bromoadiolone in biological specimens with lower concentrations.%目的 采用分子印迹同相萃取,UPLC/MS分析,检验血液中大隆和溴敌隆.方法 以大隆为模板分子,丙烯酰胺为单体,二甲基亚砜为有机溶剂,按照模板分子与单体摩尔配比关系为1:4合成大隆分子印迹聚合物,作为固相萃取剂萃取血液中大隆和溴敌隆,以2×1mL去离子水、1mL30%甲醇去离子水洗涤杂质,2 ×1mL 1%甲酸/甲醇洗脱,提取血中目标物后进行UPLC/MS分析检测.结果 溴敌隆和大隆回收率均在90%以上,在50~500ng/mL浓度范围内线性关系良好,r2溴敌隆为0.998 4,大隆为0.991,检测限(S/N=5/1)低于10ng/mL.结论 本方法回收率高,基质效应降低,杂质干扰少,可用于血液中低浓度大隆和溴敌隆的检验.

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