摘要
建立了吡啶离子液体双水相-高效液相色谱同时测定牛奶中嗯喹酸、萘啶酸及氟甲喹3种喹诺酮药物残留的方法.牛奶样品经氯化钠和磷酸混合溶液提取后,采用吡啶离子液体N-乙基-2-甲基吡啶溴化盐([EMPy]Br)和K2HPO4形成的双水相体系萃取富集,以0.1%磷酸水溶液-乙腈为流动相,梯度洗脱,紫外检测.该方法对嗯喹酸、萘啶酸和氟甲喹测定的线性范围分别为0.3—15,0.5~20和0.5~25μg/mL,相关系数(r)均大于0.9997,3种药物的检出限在8~10μg/kg之间.对不同加标浓度的牛奶样品测定,绝对回收率均在86.4%.94.8%范围内,相对标准偏差为3.6%-8.3%.该方法对牛奶中喹诺酮药物残留的检测具有简单、快速、环保和灵敏度高等优点.
A method was developed for the analysis of three quinolones ( oxolinic acid, nalidix acid and flumequine) in milk by pyridinium ionic liquid-based aqueous two-phase systems coupled with high performance liquid chromatography. Milk samples were extracted with the mixed solutions consisting of sodium chloride and phosphoric acid. Then extracts were enriched by aqueous two-phase systems composed of the ionic liquid pyri- dine N-ethyl -2-methyl-pyridine bromide salt( [ EMPy] Br) and K2HPO4. The separation of the analytes was achieved via 0. 1% phosphoric acid and acetonitrile with gradient elution under UV detection. The linear ranges are 0. 3-15μg/mL for oxolinic acid, 0. 5-20 μg/mL for nalidixic acid and 0. 5-25 μg/mL for flumequine. The correlation coefficient(r) is more than 0. 9997. The limits of detection are 8-10 μg/kg. Based on detecting spiked quinolones concentrations in milk samples, the absolute recoveries ranged from 86.4% to 94. 8% with relative standard deviation from 3.6% to 8.3%. The proposed method of determinating quinolones residues in milk is simple, rapid, friendly to environment and high sensitive.
出处
《高等学校化学学报》
SCIE
EI
CAS
CSCD
北大核心
2009年第10期1956-1959,共4页
Chemical Journal of Chinese Universities
基金
浙江省科技计划(批准号:2007C23071
2007F70011)
浙江省自然科学基金(批准号:Y4080252)
嘉兴市科技计划(批准号:2008AY2016)资助
关键词
双水相
吡啶离子液体
高效液相色谱
喹诺酮药物检测
牛奶
Aqueous two-phase systems
Pyridinium ionic liquid
High performance liquid chromatography
Determination of quinolone
Milk