色谱

色谱 ›› 2015, Vol. 33 ›› Issue (4): 434-440.DOI: 10.3724/SP.J.1123.2014.12022

• 技术与应用 • 上一篇    下一篇

高效液相色谱-柱后衍生法检测养殖水体及沉积物中11种磺胺药物残留

刘菁华, 孙振中, 黄雪玲, 郭霞, 孙建华   

  1. 上海市水产研究所, 上海市水产品质量监督检验站, 上海 200433
  • 收稿日期:2014-12-15 修回日期:2015-01-15 出版日期:2015-04-08 发布日期:2015-03-30
  • 通讯作者: 刘菁华

Determination of 11 sulfonamide residues in aquaculture water and sediments by high performance liquid chromatography coupled with post-column derivatization

LIU Jinghua, SUN Zhenzhong, HUANG Xueling, GUO Xia, SUN Jianhua   

  1. Shanghai Fisheries Research Institute, Shanghai Fisheries Technical Extension Station, Shanghai 200433, China
  • Received:2014-12-15 Revised:2015-01-15 Online:2015-04-08 Published:2015-03-30

PDF

248

被引次数

11

摘要：

建立了养殖水体及沉积物中11种磺胺化合物的高效液相色谱-柱后衍生分析方法。养殖水体过滤后采用HLB固相萃取柱进行净化、富集;沉积物采用甲醇/EDTA-Mcllvaine缓冲液(1:1, v/v)提取,HLB固相萃取柱净化富集。经高效液相色谱分离,用荧光胺衍生试剂进行柱后衍生,荧光检测器检测。对柱后衍生系统参数进行了优化,确定了荧光胺溶液的浓度、流速和反应温度分别为0.2 g/L、0.15 mL/min和50 ℃,磺胺化合物在0.01~1.0 mg/L范围内线性显著,其相关系数r2值大于0.99995。11种磺胺类药物在养殖水体和沉积物中的加标回收率分别为79.3%~100.7%和74.6%~95.3%,相对标准偏差为2.2%~11.0%和2.6%~10.3%,检出限(LOD, S/N=3)为0.9~5.5 ng/L和0.3~1.3 μg/kg,定量限(LOQ, S/N=10)为3.0~18.1 ng/L和1.0~4.4 μg/kg。该法可应用于养殖环境中磺胺类药物的定性定量检测,具有较好的实用性。

关键词: 沉积物, 高效液相色谱, 磺胺, 养殖水体, 柱后衍生

Abstract:

An analytical method was developed for the determination of 11 sulfonamide compounds in aquaculture water and sediments by high performance liquid chromatography (HPLC) coupled with post-column derivatization. The filtered water sample was purified and concentrated with HLB cartridge, while the sediment sample was extracted with a mixture of methanol and EDTA-Mcllvaine buffer (1:1, v/v), and then purified and enriched through HLB solid-phase extraction. The sulfonamides were separated on a C18 column by HPLC and on-line derivatized with a fluorescamine and detected with a fluorescence detector. The parameters of post-column derivatization system were optimized, and the fluorescamine solution concentration, velocity of reagent solution and reaction temperature were 0.2 g/L, 0.15 mL/min and 50 ℃, respectively. The calibration curves of the method showed good linearity in the range of 0.01-1.0 mg/L, with the correlation coefficients (r2) all above 0.99995. The recoveries were 79.3%-100.7% and 74.6%-95.3% with RSD values of 2.2%-11.0% and 2.6%-10.3% for the 11 sulfonamides in aquaculture water and sediments, respectively. The respective limits of detection (LODs, S/N=3) were 0.9-5.5 ng/L and 0.3-1.3 μg/kg and the limits of quantification (LOQs, S/N=10) were 3.0-18.1 ng/L and 1.0-4.4 μg/kg. The method can be applied to the determination of sulfonamides in the aquaculture environment, and it has a good practicability.

Key words: aquaculture water, high performance liquid chromatography (HPLC), post-column derivatization, sediments, sulfonamides (SAs)

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