QuEChERS-高效液相色谱-荧光法检测鸡蛋中环丙沙星、达氟沙星、恩诺沙星和沙拉沙星的残留量

Determination of quinolones residues in egg by QuEChERS and high performance liquid chromatography-fluorescence detection

中文关键词:  高效液相色谱-荧光法  环丙沙星  达氟沙星  恩诺沙星  沙拉沙星  残留  鸡蛋

英文关键词:high performance liquid chromatography-fluorescence detector  ciprofloxacin  danofloxacin  enrofloxacin  sarafloxacin  residues  egg

中文摘要:

      目的 建立QuEChERS前处理结合高效液相色谱-荧光检测器(high performance liquid chromatography-fluorescence detector, HPLC-FLD)同时检测鸡蛋中环丙沙星、达氟沙星、恩诺沙星和沙拉沙星残留量的方法。方法 鸡蛋样品添加4.0 g硫酸钠和1.0 g氯化钠, 再加入8 mL 1%甲酸乙腈进行提取, 离心后上清液再加入到Agilent dSPE净化管中, 经浓缩后采用HPLC-FLD进行检测, 0.05 mol/L磷酸三乙胺溶液(pH 2.4)-乙腈为流动相, 检测波长: 激发波长280 nm, 发射波长450 nm, 采用外标法定量。结果 环丙沙星、恩诺沙星和沙拉沙星的线性范围为2~100 μg/L, 相关系数均大于0.9999, 达氟沙星的线性范围为0.4~20 μg/L, 相关系数大于0.9999。环丙沙星、恩诺沙星、沙拉沙星的最低定量限为2 μg/kg, 达氟沙星的最低定量限为 0.4 μg/kg。环丙沙星、恩诺沙星、沙拉沙星在2~10 μg/kg的浓度添加水平上, 回收率为70.2%~91.8%, 达氟沙星在0.4~2 μg/kg的浓度添加水平上, 回收率为70.5%~96.3%, 批内、批间的相对标准偏差分别为3.89%~9.20%、5.29%~12.3%。结论 该方法简便、快速、准确、灵敏度高, 适用于鸡蛋中环丙沙星、达氟沙星、恩诺沙星和沙拉沙星残留量的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of the ciprofloxacin, danofloxacin, enrofloxacin and sarafloxacin residues in egg by QuEChERS method coupled with high performance liquid chromatography-fluorescence detector (HPLC-FLD). Methods The 4.5 g sodium sulfate and 1.0 g sodium chloride were added to the egg samples, and then 8 mL 1% acetonitrile formate was added for extraction. The supernatant was added to the Agilent dSPE purification tube after centrifugation, and the samples were detected by HPLC-FLD after concentration. The 0.05 mol/L triethylamine phosphate solution (pH 2.4)-acetonitrile was used as mobile phase, the excitation wavelength was 280 nm and the emission wavelength was 450 nm, and external standard method was used for quantification. Results Ciprofloxacin, enrofloxacin, and sarafloxacin had good relationships in the range of 2-100 ng/mL (r>0.9999), and danofloxacin in the range of 0.4-20 ng/mL (r>0.9999). The limits of quantification (LOQs) of ciprofloxacin, enrofloxacin, and sarafloxacin were 2 μg/kg, and LOQ of danofloxacin was 0.4 μg/kg. The average recoveries of ciprofloxacin, enrofloxacin, and sarafloxacin in spiked eggs at the 3 concentrations of 2, 5, and 10 μg/kg ranged from 70.2% to 91.8% (n=5), and danofloxacin in spiked eggs at the 3 concentrations of 0.4, 1, and 2 μg/kg ranged from 70.5% to 96.3% (n=5). The variation coefficients of intra-batch and inter-batch were 3.89%-9.20% and 5.29%-12.3%, respectively. Conclusion The method is simple, rapid, accurate, and sensitive, which is suitable for the determination of ciprofloxacin, danofloxacin, enrofloxacin and sarafloxacin residues in egg.