高效液相色谱法同时测定水产品中6 种喹诺酮药物的残留

doi:10.7506/spkx1002-6630-201006042

食品科学 ›› 2010, Vol. 31 ›› Issue (6): 185-189.doi: 10.7506/spkx1002-6630-201006042

高效液相色谱法同时测定水产品中6 种喹诺酮药物的残留

钱卓真^{1 , 2}，苏秀华³，魏博娟⁴，吴成业^{1 ,*}

1.福建省水产研究所 2.厦门大学材料学院 3.福建农林大学食品科学学院 4.集美大学生物工程学院

收稿日期:2009-04-29 修回日期:2009-08-24 出版日期:2010-03-15 发布日期:2010-12-29
通讯作者: 吴成业1 E-mail:wcy@fjscs.ac.cn
基金资助:
福建省地方标准渔业计划项目(闽海渔[2008]143 号)

High Performance Liquid Chromatographic Method for Simultaneous Determination of Six Quinolone Residues in Aquatic Products

QIAN Zhuo-zhen1,2，SU Xiu-hua3，WEI Bo-juan4，WU Cheng-ye1,*

1. Fisheries Research Institute of Fujian, Xiamen 361012, China；2. College of Materials, Xiamen University, Xiamen 361005,
China；3. College of Food Science, Fujian Agriculture and Forestry University, Fuzhou 350002, China；
4. College of Bioengineering, Jimei University, Xiamen 361021, China)

Received:2009-04-29 Revised:2009-08-24 Online:2010-03-15 Published:2010-12-29
Contact: WU Cheng-ye1 E-mail:wcy@fjscs.ac.cn

摘要/Abstract

摘要：

建立用固相萃取- 反相高效液相色谱法同时检测水产品中6 种喹诺酮药物残留量的方法。通过对提取方法和C18 固相萃取柱净化条件、色谱条件选择与优化、洗脱液浓度和用量的选择方面的研究，确定采用高效液相色谱分离、荧光检测器检测、外标法定量的分析方法。本方法对环丙沙星、恩诺沙星、氧氟沙星、诺氟沙星、噁喹酸、氟甲喹标准曲线的线性回归系数均在0.99 以上，线性范围为0.02～2.0μg/mL。以3 倍信噪比RSN 计算，环丙沙星、恩诺沙星、诺氟沙星、氧氟沙星检出限为2μg/kg，噁喹酸、氟甲喹检出限为5μg/kg；以10 倍信噪比RSN 计算，环丙沙星、恩诺沙星、氧氟沙星、诺氟沙星的定量下限为5μg/kg；噁喹酸、氟甲喹的定量下限为10μg/kg。在南美白对虾、罗非鱼、鳗鱼、斑点叉尾鮰中进行这6 种喹诺酮类药物加标回收率的验证实验，实验结果满意，回收率在78.8%～92.9% 之间；相对标准偏差为2.97%～7.10%。说明本方法简单、灵敏，结果可靠，可用于水产品中环丙沙星、恩诺沙星、氧氟沙星、诺氟沙星、噁喹酸、氟甲喹的同时检测。

关键词: 反相高效液相色谱法, 荧光色谱, 喹诺酮类药物, 多残留检测, 水产品

Abstract:

A solid-phase extraction followed by reversed-phase high performance liquid chromatographic (SPE-RP-HPLC) method was presented for the simultaneous determination of 6 quinolone residues (enrofloxacin, ciprofloxacin, norfloxacin, ofloxacin, oxolinic acid and flumequine) in aquatic products. Sample extraction, cleanup on a C18 cartilage column and chromatographic separation were investigated. A RP-HPLC system equipped with fluorescence detector (λex = 280 nm, λem = 480 nm) was used for analyzing 6 quinolones, and their quantification was achieved by external standard method. Six quinolones exhibited good linearity within the range of 0.02－2.0 μg/mL and the regression coefficients were all over 0.99. The developed method showed limits of detection of 2 μg/kg for ciprofloxacin, enrofloxacin, norfloxacin, ofloxacin and 5 μg/kg for oxolinic acid and flumequine (RSN = 3), and limits of quantification of 5 μg/kg for ciprofloxacin, enrofloxacin, norfloxacin, ofloxacin and 10μg/kg for oxolinic acid and flumequine (RSN = 10). Satisfying results were obtained in spike recovery experiments and average spike recoveries of 5 replicates at three levels were within the range of 78.8%－92.9%, with RSD range of 2.97%－7.10%. This method, thanks to its simplicity, sensitivity and reliability, has good suitability for the simultaneous determination of 6 quinolone residues in aquatic products.

Key words: reversed-phase high performance liquid chromatography (RP-HPLC), fluorescence spectroscopy, quinolones , multi-residue determination, aquatic products

中图分类号:

钱卓真1,2，苏秀华3，魏博娟4，吴成业1,*. 高效液相色谱法同时测定水产品中6 种喹诺酮药物的残留[J]. 食品科学, 2010, 31(6): 185-189.

QIAN Zhuo-zhen1,2，SU Xiu-hua3，WEI Bo-juan4，WU Cheng-ye1,*. High Performance Liquid Chromatographic Method for Simultaneous Determination of Six Quinolone Residues in Aquatic Products[J]. FOOD SCIENCE, 2010, 31(6): 185-189.

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高效液相色谱法同时测定水产品中6 种喹诺酮药物的残留

High Performance Liquid Chromatographic Method for Simultaneous Determination of Six Quinolone Residues in Aquatic Products

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