食品科学 ›› 2010, Vol. 31 ›› Issue (6): 248-251.doi: 10.7506/spkx1002-6630-201006059

• 分析检测 • 上一篇    下一篇

高效液相色谱法测定水产品中残留的甲氧苄啶

梅光明,陈雪昌,张小军,朱婧睿,李铁军,郑 斌*   

  1. 浙江省海洋水产研究所
  • 收稿日期:2009-05-31 修回日期:2009-10-26 出版日期:2010-03-15 发布日期:2010-12-29
  • 通讯作者: 郑 斌* E-mail:6369958@163.com

HPLC Determination of Trimethoprim Residue in Aquatic Products

MEI Guang-ming,CHEN Xue-chang,ZHANG Xiao-jun,ZHU Jing-rui,LI Tie-jun,ZHENG Bin*   

  1. (Marine Fisheries Research Institute of Zhejiang, Zhoushan 316100, China)
  • Received:2009-05-31 Revised:2009-10-26 Online:2010-03-15 Published:2010-12-29
  • Contact: ZHENG Bin* E-mail:6369958@163.com

摘要:

建立测定水产品中残留的甲氧苄啶的高效液相色谱法。样品经三氯甲烷和酸性甲醇溶液提取,提取液调至碱性后用二氯甲烷萃取,萃取液经MCX 柱净化,洗脱液浓缩至近干后用流动相溶解,过微孔滤膜,采用高效液相色谱紫外检测,外标法定量。结果表明,甲氧苄啶在0.05~5.0μg/mL 质量浓度范围内,色谱峰面积与甲氧苄啶质量浓度之间线性关系良好(相关系数为0.999967),在空白样品的20、40、200μg/kg 3 个加标量条件下,样品平均回收率均大于80%,相对标准偏差小于7%,方法的检测限为20μg/kg。该方法简便快速,基体干扰小,精密度、准确性均能满足水产品中甲氧苄啶的残留分析。

关键词: 甲氧苄啶, 水产品, 紫外检测, 高效液相色谱法

Abstract:

A reversed-phase high performance liquid chromatographic (RP-HPLC) method was developed for the determination of trimethoprim residue in aquatic products. Samples were extracted with a mixture of chloroform, sulfuric acid and methanol (15:14:6, V/V). The resulting extraction solution was alkalized, reextracted with dichloromethane and cleaned up on MCX column. The eluate was pooled, concentrated nearly to dryness, rediluted with the HPLC mobile phase and filtrated through a 0.45 μm pore size membrane. Trimethoprim was detected with an ultraviolet (UV) detector and quantified by external standard method. Good linearity between chromatographic peak area and trimethoprim concentration ranging from 0.05 to 5.0 μg/mL was found (R2 = 0.999967). Average recoveries of trimethoprim in different blank aquatic products spiked at the levels of 20, 40, 200 μg/kg were all more than 80%, with relative standard deviations of less than 7%. The method exhibited a detection limit of 20 μg/kg. Due to the advantages of simplicity, rapidity, little matrix interference and high accuracy and precision, this method is most suitable for the determination of trimethoprim residue in aquatic products.

Key words: trimethoprim, aquatic product, ultraviolet (UV) detection, high performance liquid chromatography

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