离子液体分散液相微萃取-HPLC法测定液态奶中恩诺沙星和环丙沙星  

Determination of enrofloxacin and ciprofloxacin in liquid milk by ionic liquid-based dispersive liquid-phase microextraction coupled with HPLC

作　　者：孙鹏[1,2] 乔石 郭秀娟 高玉玲[1] 

机构地区：[1]黑龙江八一农垦大学测试中心,大庆163319 [2]黑龙江大学化学化工与材料学院,哈尔滨150080 [3]威海海洋职业学院,荣成264300

出　　处：《药物分析杂志》2017年第1期111-116,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：大庆市科技计划指导项目(szdfy-2015-50);黑龙江八一农垦大学校内培育课题(XZR2014-17)

摘　　要：目的:建立一种基于离子液体的分散液相微萃取的样品前处理技术,结合高效液相色谱方法,测定液态奶中残留药物恩诺沙星和环丙沙星。方法:考察了萃取剂种类、萃取剂体积、涡旋萃取时间、盐浓度、pH因素对萃取效率的影响。确定了最佳萃取条件:以100μL 1-辛基-3-甲基咪唑六氟磷酸盐[(OMIM)PF_6]为萃取剂,氯化钠质量分数为6%,pH=3.2,涡旋震荡3 min,室温下10 000r·min^(-1)离心3 min,取20μL萃取液供高效液相色谱分析。结果:恩诺沙星和环丙沙星质量浓度在5~100μg^L^(-1)范围内与相应的峰面积呈良好的线性关系,相关系数分别为0.999 6和0.999 1;在5~20μg·L^(-1)的添加水平下,平均回收率为83.9%~98.8%,日内RSD均低于7.6%(n=6),日间RSD均低于12.1%(n=3),恩诺沙星和环丙沙星在液态奶中的检出限为0.56μg·L^(-1)和0.97μg·L^(-1),定量限为1.87μg·L^(-1)和3.23μg·L^(-1),市售液态奶样品中均未检出恩诺沙星和环丙沙星。结论:该方法操作简单,消耗试剂少,定量准确,可用于液态奶中喹诺酮类药物残留的分析检测。Objective： To establish a sample pretreatment technique based on ionic liquid-based liquid-phase microextraction （ SPME ） and to determine the residues of enrofloxacin and ciprofloxacin in liquid milk by high performance liquid chromatography （ HPLC ）. Methods： The effects of extraction solvent, volume of extractant, vortex extraction time, salt concentration and pH on extraction efficiency were investigated. The optimal extraction conditions were determined as follows： 100μL 1-octyl-3-methylimidazolium hexafluorophosphate [ （ OMIM ） PF6] as extraction solvent, the mass fraction of NaCl was 6% in sample, the pH was adjusted to 3.2. Vortex extraction lasted 3 min, and centrifugal time was 3 rain in room temperature centigrade at rate of 10 000 r·min-1, and 20μL extraction solvent was obtained from the sample with micro sample feeder for HPLC. Results： The calibration curves of enrofloxaein and ciprofloxaein were linear in the range of 5.0 to 100 μg· L-1 with the correlation coefficients of 0. 999 6 and 0. 999 1, respectively. The average recoveries of enrofloxacin and ciprofloxacin in liquid milk were in the range of 83.9% to 98.8% at spiked levels of 5 to 20 μg·L-1, with intra- day relative standard deviations lower than 7.6% （ n=6 ） and inter-day relative standard deviations lower than 12. 1% （ n=3 ）. The limits of detection and quantification were 0. 56 μg·L-1 and 97 μg·L-1, and the limits of quantification were 1.87 μg·L-1 and 3.23 μg·L-1, respectively. Enrofloxacin and ciprofloxacin were not detected in liquid milk. Conclusion： The established method is simple, solvent saving, accurate and can be used for the residual analysis of enrofloxacin and ciprofloxacin in liquid milk sample.

关 键 词：喹诺酮 离子液体 兽药残留 样品富集 分散液相微萃取 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]