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作 者:汪雪雁[1] 祁克宗[2] 檀华蓉[3] 魏传宇[1]
机构地区:[1]安徽农业大学茶与食品科技学院,合肥230036 [2]安徽农业大学动物科技学院,合肥230036 [3]安徽农业大学生物技术中心,合肥230036
出 处:《安徽农业大学学报》2012年第6期867-870,共4页Journal of Anhui Agricultural University
基 金:国家十一五科技支撑项目子项目(2006BAK02A08-4)资助
摘 要:建立了固相萃取-高效毛细管电泳同时分离达氟沙星、恩诺沙星和培氟沙星3种氟喹诺酮类药物的方法,并对来自于安徽33个牧场的165组牛奶样品进行检测。研究了缓冲液离子浓度、pH、分离电压以及温度等电泳参数,最终通过正交试验得到最佳分离条件:紫外检测波长215 nm,缓冲液为40 mmol·L-1磷酸氢二钾~20mmol·L-1柠檬酸冲溶液体系,pH8.10,检测电压20 kV,检测温度25℃。结果表明,3种药物在7 min内完全分离,各组分浓度与峰面积呈良好的线性关系,R2为0.997 7-0.999 7;试验平均回收率在71.00%-84.58%之间,RSD为0.22%-0.67%(迁移时间)和5.41%-9.75%(峰面积)。165组鲜牛奶中3种氟喹诺酮类药物的检出率为9.1%。安徽省奶源存在一定程度的氟喹诺酮药物残留,需要加强对牧场的监测和管理力度。A method for the simultaneous separation of fluoroquinolones(FQs) by solid phase extraction (SPE) & high performance capillary electrophoresis (HPCE) was developed, and in this way, 165 samples from 33 large-scale farms in Anhui were determined. The effects of several factors such as the ion concentration, pH value of running buffer, the voltage and the temperature on separation of samples were investigated. The optimal condition was found by orthogonal experiment. The optimal conditions were as follows. UV detection wavelength, 215 nm; running buffer, 40 mmol·L-1 Na2HPO4- 20 mmol·L-1 citric acid; pH 8.10; separation voltage, 20 kV, The results showed that the fluoroquinolones residues can be separated within 7 min, and each had a good linear relationship between concentration and peak area (R2=0.997 7-0.9997) .The average recoveries were between 71.00%-84.58%%. The RSDs were 0.22%-0.67 %( transition time) and 5.41%-9.75 %( peak area). The positive rate was 9.1%, and the method for detection of antibiotic FQs in large-scale farms of Anhui was set up. The monitoring and management on milk-producing households should be enhanced.
关 键 词:牛奶 氟喹诺酮类药物 固相萃取 高效毛细管电泳 残留
分 类 号:S859.84[农业科学—临床兽医学] R155.57[农业科学—兽医学]
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