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›› 2017, Vol. 39 ›› Issue (5): 386-391.

• 论文与报告 • 上一篇    下一篇

全自动固相萃取-超高效液相色谱法测定淡水养殖水体中的呋喃丹

牛曰华   

  1. 福建省海洋环境与渔业资源监测中心
  • 收稿日期:2017-08-03 修回日期:2017-08-24 出版日期:2017-10-25 发布日期:2017-11-02
  • 通讯作者: 牛曰华

Determination of carbofuran in freshwater aquaculture water by ultra high performance liquid chromatography with automatic solid phase extraction

  • Received:2017-08-03 Revised:2017-08-24 Online:2017-10-25 Published:2017-11-02

摘要: 本文建立了淡水养殖水体中呋喃丹的全自动固相萃取-超高效液相色谱检测方法。选取HLB固相萃取小柱作为水样的富集和净化小柱,水样以5 mL·min-1的速度上样,用10 mL甲醇洗脱。洗脱液经浓缩、定容后,用超高效液相色谱-荧光检测法分析,色谱柱为ACQUITY UPLC BEH C18柱(100 mm × 2.1 mm,粒径1.7 μm),流动相为乙腈-水(40∶60,V/V),流速为0.200 mL·min-1,激发波长为270 nm,发射波长为310 nm。呋喃丹在20~1 000 μg·L-1范围内线性关系良好,相关系数R2 > 0.999,方法检出限为0.100 μg·L-1,定量限为0.250 μg·L-1,在0.250、2.50、10.0 μg·L-1三种加标浓度水平下,平均加标回收率为90.4% ~ 96.3%,相对标准偏差为2.55% ~ 5.10%。该方法自动化程度高、操作简便、快速准确、稳定性好,适用于淡水养殖水体中呋喃丹的测定。

关键词: 呋喃丹, 超高效液相色谱, 全自动固相萃取, 淡水养殖水体, carbofuran, ultra high performance liquid chromatography, automatic solid phase extraction, freshwater aquaculture water

Abstract: A new method was developed for the determination of carbofuran in freshwater aquaculture water by ultra high pressure liquid chromatography (UPLC) combined with automatic solid phase extraction (SPE). The water sample flowed through HLB SPE cartridge with a flow rate of 5 mL·min-1, and the analyte was eluted with 10 mL methanol in SPE cartridge. After concentrating and redissolving with acetonitrile-water (40∶60, V/V), the eluent was analyzed by ultra high performance liquid chromatography with fluorescence detection. The analysis conditions were as the follows: chromatographic column: ACQUITY UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm), mobile phase: acetonitrile-water (40∶60, V/V), flow rate: 0.200 mL·min-1, excitation wavelength: 270 nm, emission wavelength: 310 nm. The correlation coefficients of carbofuran standard curve was more than 0.999 in the range of 20 ~ 1000 μg·L-1. The limit of detection was 0.10 μg·L-1 and the limit of quantitation was 0.25 μg·L-1. The average recoveries were in the range of 90.4% ~ 96.3% and the relative standard deviations were 2.55% ~ 5.10% at 0.25 μg/L, 2.50 μg·L-1 and 10.0 μg·L-1 spiked levels. The method is highly automated, simple, rapid, accurate and stable, and is suitable for the determination of carbofuran in freshwater aquaculture water.

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