| 摘要: |
| 建立了鸡蛋中环丙沙星、达氟沙星、恩诺沙星和沙拉沙星4种氟喹诺酮类药物残留测定的超高效液相色谱方法。样品经磷酸盐缓冲液提取后,用正己烷脱脂,C18固相萃取柱净化,反相高效液相色谱分离,荧光检测器测定。本方法的检测限为环丙沙星、恩诺沙星和沙拉沙星5 μg/kg,达氟沙星1 μg/kg。环丙沙星、恩诺沙星和沙拉沙星在2~200 ng/mL、达氟沙星在0.4～40 ng/mL范围内呈线性相关,相关系数r大于0.9999。在空白鸡蛋中添加环丙沙星、恩诺沙星和沙拉沙星5~50 μg/kg、达氟沙星1～10 μg/kg,4种氟喹诺酮类药物的平均回收率为82.2～101.3％,批内变异系数0.8～5.9％之间(n＝6),批间变异系数在1.0～6.6％之间(n＝4)。结果表明,该法灵敏、准确、特异性强,适用于鸡蛋中氟喹诺酮类药物残留的测定。 |
| 关键词: 鸡蛋 氟喹诺酮类药物 残留 高效液相色谱 |
| DOI： |
| 投稿时间：2021-03-01修订日期：2021-09-01 |
| 基金项目: |
|
| Optimization of the Pretreatment Method for the Determination of Fluoroquinolones Residues in Eggs by High Performance Liquid Chromatography |
|
| (Henan Institute of Veterinary Drug and Feed Control,Zhengzhou,450008) |
| Abstract: |
| An ultra-high performance liquid chromatography method for testing ciprofloxacin, danofloxacin, enrofloxacin and sarafloxacin residues in eggs was established. After the sample was extracted with phosphate buffer, it was degreased with n-hexane, and purified with C18 solid phase extraction column, separated by reversed-phase HPLC, and measured by fluorescence detector. The detection limit of this method is 5 μg/kg for ciprofloxacin, enrofloxacin and sarafloxacin, and 1 μg/kg for danofloxacin. Ciprofloxacin, enrofloxacin and sarafloxacin were linearly correlated in the range of 2~200 ng/mL, and danofloxacin were linearly correlated in the range of 0.4-40 ng/mL, the correlation coefficient r was greater than 0.9999. Adding 5-50 μg/kg of ciprofloxacin, enrofloxacin and sarafloxacin, 1-10 μg/kg of danofloxacin to blank eggs sample, the average recovery rate of the four fluoroquinolones is 82.2-101.3%, the intra-assay coefficient of variation is between 0.8 and 5.9% (n=6), and the inter-assay coefficient of variation is between 1.0 and 6.6% (n=4). The results indicated that the method is sensitive, accurate and specific, and is suitable for the testing of fluoroquinolones residues in eggs. |
| Key words: Eggs Fluoroquinolones Residues High Performance Liquid Chromatography |
