高效液相色谱法测定鸡蛋中氟喹诺酮类药物残留量前处理方法的优化

Optimization of the Pretreatment Method for the Determination of Fluoroquinolones Residues in Eggs by High Performance Liquid Chromatography

关键词:  鸡蛋  氟喹诺酮类药物  残留  高效液相色谱

Key words:  Eggs  Fluoroquinolones  Residues  High Performance Liquid Chromatography

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。

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.