食品科学

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超高效液相色谱法测定水体和沉积物中4 种硝基呋喃类抗生素

王 强,王旭峰,赵东豪,黄 珂,黎智广,李永贤,杨宏亮,李刘冬   

  1. 中国水产科学研究院南海水产研究所,农业部水产品加工重点实验室,
    农业部水产品贮藏保鲜质量安全风险评估实验室,广东 广州 510300
  • 出版日期:2016-08-25 发布日期:2016-08-30
  • 通讯作者: 李刘冬
  • 基金资助:

    国家农产品质量安全风险评估重大专项(GJFP2014009);
    中央级公益性科研院所基本科研业务费专项(2013TS08;2014TS09;2015TS17;2015TS18)

Determination of Four Nitrofurans in Water and Sediment Using Ultra Performance Liquid Chromatography

WANG Qiang, WANG Xufeng, ZHAO Donghao, HUANG Ke, LI Zhiguang, LI Yongxian, YANG Hongliang, LI Liudong   

  1. South China Sea Fisheries Research Institute, Key Laboratory of Aquatic Product Processing, Ministry of Agriculture,
    Laboratory of Quality and Safety Risky Assessment for Aquatic Product on Storage and Preservation, Ministry of Agriculture,
    Chinese Academy of Fishery Sciences, Guangzhou 510300, China
  • Online:2016-08-25 Published:2016-08-30
  • Contact: LI Liudong

摘要:

建立超高效液相色谱法同时测定水体和沉积物中的呋喃妥因、呋喃西林、呋喃它酮和呋喃唑酮4 种硝基呋喃类抗生素。水体样品过滤后直接用混合型阳离子交换(mixed-mode cation exchange,MCX)固相萃取柱富集净化;沉积物样品经乙腈-0.1%甲酸溶液(8∶2,V/V)提取,MCX固相萃取柱净化。采用BEH C18(100 mm×2.1 mm,1.7 μm)色谱柱分离,以0.1%甲酸溶液-乙腈为流动相梯度洗脱。4 种硝基呋喃类药物在10.0~200 μg/L质量浓度内范围线性关系良好,相关系数R2均大于0.999。水体和沉积物中的加标回收率分别为81.5%~103.2%和73.3%~91.9%,相对标准偏差分别为2.0%~5.8%和3.4%~9.6%(n=5),检出限分别为0.03 μg/L和0.6 μg/kg,定量限分别为0.1 μg/L和2.0 μg/kg。该方法可应用于水体和沉积物中硝基呋喃类抗生素的残留检测。

关键词: 超高效液相色谱, 水体, 沉积物, 硝基呋喃

Abstract:

An ultra performance liquid chromatography (UPLC) method was developed for the simultaneous determination
of 4 nitrofuran antibiotics (furazolidone, furaltadone, nitrofurazone and nitrofurantion) in water and sediment. Water
samples were filtrated and cleaned up using mixed-mode cation exchange solid-phase extraction column (MCX). Sediment
samples were extracted with acetonitrile-0.1% formic acid solution (8:2, V/V), and then cleaned up also with MCX solidphase
extraction column. The analytes were separated on a BEH C18 column (100 mm × 2.1 mm, 1.7 μm) utilizing gradient
elution with a mixture of acetonitrile and 0.1% formic acid solution as the mobile phase. The method showed good linearity
in the range of 10.0–200 μg/L with correlation coefficients (R2) all above 0.999. The recoveries were 81.5%–103.2% and
73.3%–91.9% with relative standard deviations (RSDs, n = 5) of 2.0%–5.8% and 3.4%–9.6% for 4 nitrofurans in water and
sediment, respectively. The limits of detection (LODs) were 0.03 μg/L and 0.6 μg/kg and the limits of quantitation (LOQ)
were 0.1 μg/L and 2.0 μg/kg, respectively. The method can be applied to the determination of nitrofuran antibiotics residues
in water and sediment.

Key words: ultra performance liquid chromatography (UPLC), water, sediment, nitrofuran

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