PDF《孙鹏 1,》

・111・ 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 * 孙鹏 1,

2 , 乔石

3 , 郭秀娟

3 , 高玉玲 1** (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) 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100μ L 1- 辛基 -3- 甲基咪唑六氟磷酸盐 [ (OMIM) PF6] 为萃取剂, 氯化钠质量分数为6%, pH=3.2, 涡旋震荡3min, 室温下10

000 r・min-1 离心3min, 取20 μL 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 5~100 μg・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5~20 μg・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 0.56 μg・L-1 和0.97 μg・L-1 , 定量限为 1.87 μg・L-1 和3.23 μg・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. 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 中图分类号: R

917 文献标识码: A 文章编号: 0254-1793 (2017) 01-0111-06 doi: 10.16155/j.0254-1793.2017.01.14 Determination of enrofloxacin and ciprofloxacin in liquid milk by ionic liquid-based dispersive liquid-phase microextraction coupled with HPLC* SUN Peng1,

2 , QIAO Shi3 , GUO Xiu-juan3 , GAO Yu-ling1** (1.Testing Centre, Heilongjiang Bayi Agricultural University, Daqing 163319, China;

2.School of Chemistry and Materials Science, Heilongjiang University, Harbin 150080, China, 3.Weihai Ocean Vocational College, Rongcheng 264300, China) Abstract 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 * 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) ** 通信作者 Tel: (0459) 2673842;

E-mail: [email protected] 第一作者 Tel: (0459) 6819128;

E-mail: [email protected] ・112・ 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 min in room temperature centigrade at rate of

10 000 r・min-1 , and

20 μL extraction solvent was obtained from the sample with micro sample feeder for HPLC. Results: The calibration curves of enrofloxacin and ciprofloxacin 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