高效液相色谱法同时测定水产品中多种氟喹诺酮类药物残留量

Simultaneous determination of multi-fluoroquinolones residues in aquatic products by HPLC

本文建立了一种同时测定水产品中多种氟喹诺酮类药物残留量的高效液相色谱法。样品经酸性乙腈提取,正己烷液-液分配净化,0.01mol·L-1四丁基溴化铵溶液溶解残渣,过微孔滤膜,采用高效液相色谱附荧光检测器检测,外标法定量。氧氟沙星、环丙沙星、恩诺沙星线性范围为0.002～0.200μg·mL-1;诺氟沙星、达氟杀星线性范围为0.001～0.100μg·mL-1,5种氟喹诺酮类药物的相关系数为0.99901～0.99917;在0.002～0.040mg·kg-1浓度范围内,样品平均加标回收率在75.6%～98.3%之间,相对标准偏差为3.45%～10.01%;方法的最低检出限氧氟沙星、诺氟沙星、环丙沙星、恩诺沙星、达氟沙星分别为0.004、0.002、0.004、0.004、0.002mg·kg-1。

A high performance liquid chromatographic method was developed for the determination of multifluoroquinolones residues in aquatic products.The fluoroquinolone residues in the test sample are extracted with acidic acetonitrile.The residues are cleaned up with n-hexane.The residues are dissolved with 0.01mol·L^-1 tetrabutylammonium bromide, filtered through a 0.45 μm membrane and determined by HPLC with FLD-detector, using external standard method.The liner range was 0.002 ～0.200μg·mL^-1 for ofloxacin , ciprofloxacin and enrofloxacin, 0.001 ～0.100μg·mL^-1 for norfloxacin and danofloxacin.The correlation coefficients were 0.99901 ～ 0.99917 for the five fluoroquinolones.The average recoveries of five fluoroquinolones in spiked chicken ranged from 75.6%～98.3%, and the relative standard deviations were between 3.45%～10.01% at spiked levels of 0.002～ 0.040mg·kg^-1.The limit of detection was 0.004mg·kg^-1 for ofloxacin , ciprofloxacin and enrofloxacin, 0.002mg·kg^-1 for norfloxacin and danofloxacin.