超声辅助-离子液体分散液液微萃取-高效液相色谱法测定液态奶中3种四环素类抗生素的残留  

Determination of 3 Tetracyclines Residues by Ultrasound-assisted Ionic Liquid Dispersive Liquid-liquid Microextraction Coupled with High Performance Liquid Chromatography in Liquid Milk

作　　者：孙鹏[1] 高玉玲[1] 王爽[1] 

机构地区：[1]黑龙江八一农垦大学测试中心,黑龙江大庆163319

出　　处：《化学试剂》2016年第10期999-1002,1007,共5页Chemical Reagents

基　　金：大庆市指导性科技计划项目(szdfy-2015-50);"校内培育课题资助计划"项目(XZR2014-17)

摘　　要：建立了一种超声辅助离子液体分散液液微萃取样品前处理技术,结合高效液相色谱法测定液态奶中3种四环素类抗生素药物的残留。考察了萃取剂种类、萃取剂体积、分散剂种类、超声萃取时间、萃取温度、盐浓度等因素对萃取效率的影响。确定了最佳萃取条件：80μL 1-辛基-3-甲基咪唑六氟磷酸盐（[OMIM]PF6）为萃取剂,800μL甲醇为分散剂,Na Cl质量分数为10%,35℃下,超声萃取30 min。结果表明,3种四环素类抗生素药物在5~150μg/L范围内呈良好的线性关系,线性相关系数为0.998 8~0.999 4,检出限为0.36~1.21μg/L,加标回收率为86.5%~98.8%,RSD为6.5%~9.7%。该方法简单、高效、安全,可用于液态奶中四环素类抗生素药物残留的分析检测。A novel method for the determination of 3 tetracyclines residues from the liquid milk has been developed using ultra- sound-assisted ionic liquid dispersive liquid-liquid microextraction coupled with high performance liquid chromatography. The in- fluence of extraction parameters including types of extraction solvent, volume of extraction solvent, ultrasonic extraction tempera- ture, ultrasonic extraction time,types of dispersant solvent,NaCl mass fraction were investigated. Using 80μL 1-octyl-3-methylimi- dazolium hexafluorophosphate （[ OMIM ] PF6 ） as extraction drop,800 μL methanol as dispersant solvent, NaCl mass fraction 10% ,extraction temperature 35℃ ,ultrasonic extraction 30 min. Under the optimal conditions,good linear relationships were ob- tained in the three tetracyelines residues concentrations of 5 - 150 μg/L with the correlation coefficients of 0. 998 8 - 0. 999 4. The detection limits were 0. 36 - 1.21μg/L. The proposed method was used to the determination of three tetracyclines residues in liquid milk, the recoveries were from 86. 5% to 98.8% ,with the corresponding RSD were from 6.5 % to 9.7%. The method was considered to be simple, fast,and precise to satisfy the requirements of the residual analysis of tetracyclines.

关 键 词：超声辅助 离子液体 抗生素 超高效液相色谱 分散液液微萃取 

分 类 号：O658.2[理学—分析化学]