Citation: HUANG Dongmei, HUANG Xuanyun, GU Runrun, HUI Yunhua, TIAN Liangliang, FENG Bing, ZHANG Xuan, YU Huijuan. Determination of 14 sulfonamide residues in shrimps by high performance liquid chromatography coupled with post-column derivatization[J]. Chinese Journal of Chromatography, ;2014, 32(8): 874-879. doi: 10.3724/SP.J.1123.2014.04009 shu

Determination of 14 sulfonamide residues in shrimps by high performance liquid chromatography coupled with post-column derivatization

1.
East China Sea Fisheries Research Institute, Chinese Academy of Fisheries Sciences, Shanghai 200090, China

Corresponding author: YU Huijuan,
Received Date: 3 April 2014
Available Online: 8 July 2014
Fund Project: 中央级公益性科研院所基本业务费专项基金(中国水产科学研究院)资助项目(2012A1003). (中国水产科学研究院)资助项目(2012A1003)

A method for the determination of 14 sulfonamide residues in shrimps by high performance liquid chromatography coupled with post-column derivatization was established. The sulfonamide residues were extracted with ethyl acetate after adding sulfapyridine as internal standard. The extracts were vacuum-concentrated and reverse-extracted by 2 mol/L hydrochloric acid solution for clean-up, and then the hydrochloric acid solution was defatted with n-hexane. The solution after filtration was blended with a mixed solution of methanol, acetonitrile and 3.5 mol/L sodium acetate solution (5:5:20, v/v/v). The sulfonamides were separated on a C₁₈ column by RP-HPLC and on-line derivatized with a fluorescamine and detected with a fluorescence detector. The standard addition method was used for quantitative analysis. The parameters of post-column derivatization system, such as concentration of fluorescamine solution, velocity of reagent solution and reaction temperature, were optimized. The calibration curves of the method showed good linearity in the range of 5-200 μg/L. The limits of quantification (LOQ, S/N=10) were 1.0-5.0 μg/kg for the 14 sulfonamides. The recoveries were 77.8%-103.6% in the spiked range of 1.0-100.0 μg/kg in shrimps with the relative standard deviations of 2.9%-9.1% (n=6). The results indicated that the method is sensitive, efficient and more accurate. It is suitable for the simultaneous determination of the 14 sulfonamide residues in shrimps.
- high performance liquid chromatography (HPLC),
- post-column derivation,
- fluorescence detection,
- sulfonamides,
- shrimps,
- fluorescamine,
- residues
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沈阳化工大学材料科学与工程学院沈阳 110142