摘要
旨在建立一种利用高效液相色谱仪检测牛奶中氟喹诺酮类药物的多残留的方法。在酸性介质中用乙腈提取牛奶中的目标化合物,用正已烷进行脱脂,提取液经浓缩后,用流动相溶解,利用高效液相色谱仪进行测定[1-3]。试验结果表明:恩诺沙星、环丙沙星、沙拉沙星、二氟沙星浓度在5~500 ng/mL,达氟沙星在1~100 ng/mL范围时与峰面积呈良好的线性关系,相关系数均大于0.9999。检测限恩诺沙星、环丙沙星、沙拉沙星、二氟沙星为5 ng/mL,定量限为10 ng/mL。达氟沙星检测限为1 ng/mL,定量限为2 ng/mL。恩诺沙星、环丙沙星、沙拉沙星、二氟沙星在10~100 ng/mL的浓度添加水平上,平均回收率均在70.3%~94.0%(n=6)之间,达氟沙星在2~20 ng/mL的浓度添加水平上,平均回收率均在73.5%~88.8%(n=6)之间。批内、批间变异系数均小于12.0%。试验结果说明:该方法具有重现性好,操作简便、精确的特点,可用于牛奶中氟喹诺酮类药物的测定。
The aim of this study was to establish a method for determination of fluroquinolones residues in milk with HPLC.The target compounds in milk were extracted with acetonitrile in an acidic medium and degreased with n-hexane.After concentration,the extract was dissolved in mobile phase and determined by HPLC.Results showed that there was a good linear relationship between the peak area and the concentration at the range of 5 to 500 ng/mL(enrofloxacin,ciprofloxacin,sarafloxacin,difloxacin)and of 1 to 100 ng/mL(danofloxacin),and the correlation coefficients were all greater than 0.9999.The detection limit of the method for danofloxacin was 1 ng/mL and the detection limits for the others were all 5 ng/mL.The quantification limit of the method for danofloxacin was 2 ng/mL,and the limits for the others were all 10 ng/mL.The average recovery of danofloxacin at the concentrations of 2 to 20 ng/mL ranged from 73.5%to 88.8%(n=6),and the recoveries of the others at the concentrations of 10 to 100 ng/mL ranged from 70.3%~94.0%(n=6).The coefficients of variation within and between batches were both less than 12.0%.As a result,the method had the characteristics of good reproduciblity,simple operation and accuracy,it could be used for the determination of fluroquinolones in milk.
作者
宫秀杰
萨仁高娃
阿力腾才斯克
史梅
GONG Xiu-jie;SARENGAOWA;ALITENGCAISIKE;SHI Mei(Xinjiang Institute for Veterinary Drugs and Feedstuff Control,Urumqi,830063,China)
出处
《草食家畜》
2020年第4期57-62,共6页
Grass-Feeding Livestock
