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

发布时间：2018-03-05 04:06

本文选题：喹诺酮　切入点：离子液体　出处：《药物分析杂志》2017年01期 　论文类型：期刊论文

【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。
[Abstract]:Objective: to establish a sample pretreatment technique based on ionic liquid dispersible liquid microextraction and to determine the residual drugs enrofloxacin and ciprofloxacin in liquid milk by high performance liquid chromatography. The optimum extraction conditions were determined as follows: 100 渭 L 1-octyl -3-methyl imidazolium hexafluorophosphate [OMIMN PF6] as extractant. The mass fraction of sodium chloride was 6 渭 m pH ~ (-2), vortex oscillating for 3 min, centrifugation at room temperature (10 000 r 路min ~ (-1)) for 3 min, and 20 渭 L extract was used for HPLC analysis. Results: the linear relationship between the concentration of enrofloxacin and ciprofloxacin in the range of 5 ~ 100 渭 g / L ~ (-1) showed a good linear relationship with the corresponding peak area, and a good linear relationship was found between the concentration of enrofloxacin and ciprofloxacin in the range of 5 ~ 100 渭 g / L ~ (-1). The correlation coefficients were 0.999 6 and 0.999 1, respectively, at the addition level of 5 ~ 20 渭 g 路L ~ (-1), The average recovery rate was 83.9 渭 g 路L ~ (-1). The average recovery rate was 83.9 渭 g 路L ~ (-1). The average daily RSD was lower than 7.66 渭 g 路L ~ (-1). The daytime RSD was lower than 12.1g 路L ~ (-1). The detection limits of enrofloxacin and ciprofloxacin in liquid milk were 0.56 渭 g 路L ~ (-1) and 0.97 渭 g 路L ~ (-1) with a quantitative limit of 1.87 渭 g 路L ~ (-1) and 3.23 渭 g 路L ~ (-1). Conclusion: this method is simple to operate, It can be used for the determination of quinolones residues in liquid milk.
【作者单位】：黑龙江八一农垦大学测试中心;黑龙江大学化学化工与材料学院;威海海洋职业学院;
【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)
【分类号】：R155.5

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