基于低毒溶剂的MSPD/HPLC法同时测定鱼肉中8种磺胺类药物残留

doi:10.7506/spkx1002-6630-200904036

食品科学 ›› 2009, Vol. 30 ›› Issue (4): 178-181.doi: 10.7506/spkx1002-6630-200904036

基于低毒溶剂的MSPD/HPLC法同时测定鱼肉中8种磺胺类药物残留

赵海香^1,2,3，邓维²，尚艳芬²，赵孟彬²，丁明玉^1,*

1.清华大学化学系 2.中关村海淀园北京锦绣大地农业股份有限公司博士后工作站 3.河北北方学院基础农学部

收稿日期:2008-03-11 修回日期:2008-09-26 出版日期:2009-02-15 发布日期:2010-12-29
通讯作者: 赵海香 E-mail:xzhaoh@126.com
基金资助:
北京市海淀区科委企业博士后科研专项(k2008198)

Simultaneous Determination of Eight Sulfonamide Residues in Fish Muscle Using Matrix Solid-phase Dispersion Coupled with High Performance Liquid Chromatography Based on Low Toxic Solvent

ZHAO Hai-xiang1,2,3，DENG Wei2，SHANG Yan-fen2，ZHAO Meng-bin2，DING Ming-yu1,*

(1. Department of Chemistry, Tsinghua University, Beijing 100084, China；2. Enterprise Postdoctoral Workstation, Beijing
Glorious Land Agricultural Co. Ltd., Zhongguancun (Haidian) Science Park, Beijing 100049, China；3. Department of Basic
Agricultural Science, Hebei North University, Zhangjiakou 075131, China)

Received:2008-03-11 Revised:2008-09-26 Online:2009-02-15 Published:2010-12-29
Contact: ZHAO Hai-xiang1,2,3 E-mail:xzhaoh@126.com

摘要/Abstract

摘要：

本实验以基质固相分散(MSPD)和高效液相色谱(HPLC)为基础，采用低毒的乙酸乙酯为洗脱溶剂，建立了与环境友好的鱼肉组织中8 种磺胺类药物多残留快速分析法。将0.5g 鱼肉与适量C18 填料混合，研磨，制成半固态装柱，磺胺类药物经乙酸乙酯洗脱浓缩，用反相高效液相色谱测定。采用C18 柱，柱温30℃；50mmol/L NaH2PO4-乙腈(70:30，V/V)为流动相，流速0.7ml/min；紫外检测(λ =270nm)。8 种磺胺被有效分离，在0.010～1.000μg/ml范围内线性相关系数在0.9999 以上；添加回收率为76.0%～115.0%，RSD < 6.4%(n=6)；仪器检测限均为0.010μg/ml；方法检测限为0.020μg/g。

关键词: 高效液相色谱法, 鱼肉, 基质固相萃取(MSPD), 低毒溶剂, 磺胺类药物残留

Abstract:

A multi-residue analytical method for eight sulfonamides in fish muscle based on matrix solid-phase dispersion (MSPD) coupled with high performance liquid chromatography (HPLC) was developed. This method was environmentally friendly using ethyl acetate as the elution solvent. 0.5 g of fish muscle mixed with 2 g of C18 packing material was grounded and filled into a SPE column. After washing with hexane, sulfonamides were eluted with ethyl acetate and determined using RP-HPLC with UV detector at 270 nm. Sulfonamides were separated on C18 column using 50 mmol/L NaH2PO4-acetonitrile (70:30, V/V) as mobile phase at a flow rate of 0.7 ml/min, and the column temperature was 30 ℃. The linear range of this method is from 0.010 μg/ml to 1.000 μg/ml with the correlation coefficient of over 0.9999. The spike recoveries are in the range of 76.0% to 115.0% and the relative standard deviation (RSD) is less than 6.4% (n = 6). The limit of detection is 0.020 μg/g in a 0.5 g of sample.

Key words: HPLC, fish muscle, MSPD, low toxic solvent, sulfonamide residues

中图分类号:

TS207.5

赵海香1,2,3，邓维2，尚艳芬2，赵孟彬2，丁明玉1,*. 基于低毒溶剂的MSPD/HPLC法同时测定鱼肉中8种磺胺类药物残留[J]. 食品科学, 2009, 30(4): 178-181.

ZHAO Hai-xiang1,2,3，DENG Wei2，SHANG Yan-fen2，ZHAO Meng-bin2，DING Ming-yu1,*. Simultaneous Determination of Eight Sulfonamide Residues in Fish Muscle Using Matrix Solid-phase Dispersion Coupled with High Performance Liquid Chromatography Based on Low Toxic Solvent[J]. FOOD SCIENCE, 2009, 30(4): 178-181.

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基于低毒溶剂的MSPD/HPLC法同时测定鱼肉中8种磺胺类药物残留

Simultaneous Determination of Eight Sulfonamide Residues in Fish Muscle Using Matrix Solid-phase Dispersion Coupled with High Performance Liquid Chromatography Based on Low Toxic Solvent

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