SPE-HPLC法测定鳗鲡中13种磺胺类药物

福建水产 ›› 2012, Vol. 34 ›› Issue (5): 375-381.

SPE-HPLC法测定鳗鲡中13种磺胺类药物

牛曰华

福建省海洋环境与渔业资源监测中心

收稿日期:2011-06-11 修回日期:2012-06-20 出版日期:2012-10-25 发布日期:2012-10-22
通讯作者: 牛曰华

Determination of 13 sulfonamides in eels with solid phase extraction and high performance liquid chromatographic

Received:2011-06-11 Revised:2012-06-20 Online:2012-10-25 Published:2012-10-22

摘要/Abstract

摘要： 针对鳗鲡基质油脂较多的的特点，建立了一种同时测定鳗鲡中13种磺胺类药物残留的固相萃取-高效液相色谱方法。样品用乙酸乙酯提取，浓缩后用盐酸溶解，正己烷除脂，经混合型阳离子交换固相萃取柱净化后，用高效液相色谱分离，DAD检测器检测，外标法定量。13种磺胺类药物在0.01 ~ 2.0 ug/mL范围内线性关系良好，相关系数R2 ≥ 0.9999，平均加标回收率为 71.7% ~ 89.8%，相对标准偏差为0.80% ~ 7.82%。方法检出限为3.05 ~ 5.24 μg/kg，定量限为10.1 ~ 17.5 μg/kg。

关键词: 磺胺类药物, 混合型阳离子交换固相萃取柱, 高效液相色谱, 鳗鲡, sulfonamides, mixed mode cation exchange solid phase extraction column, high performance liquid chromatographic, eel

Abstract: A solid phase extraction and high performance liquid chromatographic method has been developed for the simultaneous determination of thirteen sulfonamides residues in eel products.The samples were extracted with ethyl acetate,concentrated and dissolved with hydrochloric acid ,then cleaned up by n-hexane liquid -liquid extraction and solid phase extraction.The residues were determined by high performance liquid chromatography with diode array detector and quantified by external standard method.The linear ranges were 0.01~2.0 mg/L with the correlation coefficient over 0.9999.The average recoveries in spiked samples were found to be in the range of 71.7%~89.8% with relative standard deviation of 0.80%~7.82%. The limits of detection were found to be 3.05 ~5.24 μg/kg and the limits of quantification 10.1 ~ 17.5 μg/kg.

中图分类号:

O657.7

牛曰华. SPE-HPLC法测定鳗鲡中13种磺胺类药物[J]. 福建水产, 2012, 34(5): 375-381.

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