ASE-GPC-HPLC法同时测定水产品中13种磺胺类和甲氧苄啶的残留  

Simultaneous determination of 13 kinds of sulfonamides and trimethoprim residues of aquatic products by ASE-GPC-HPLC method

作　　者：王静 沈吴琪[3] 张美琴[1,2] 孟勇[1,2] 吴光红[1,2] 

机构地区：[1]江苏省水产质量检测中心,江苏南京210017 [2]江苏省淡水水产研究所,江苏南京210017 [3]中国药科大学药学院,江苏南京211198

出　　处：《水产学报》2013年第8期1244-1249,共6页Journal of Fisheries of China

基　　金：海洋水产品食品加工技术研发与产业化示范项目(2012BAD28B05)

摘　　要：为了开发一种以加速溶剂萃取、全自动凝胶渗透色谱、高效液相色谱联用(ASE-GPC-HPLC)来同时测定水产品中13种磺胺类和甲氧苄啶残留的方法,实验采用凡纳滨对虾等水产品通过加速溶剂萃取仪提取,经全自动凝胶渗透色谱仪净化,收集液经氮吹浓缩后用1 mL流动相定容,HPLC检测,外标法定量。结果显示,13种磺胺类在0.01～1.00 mg/L范围内、甲氧苄啶在0.02～2.00 mg/L范围内线性关系良好,相关系数均>0.999 9;添加100、200、400μg/kg 3个浓度水平的平均回收率为77.9%～98.6%,RSD为0.4%～13.4%。研究表明,运用ASE的提取优势和GPC的净化效果提高了检测结果的回收率和精密度,降低基质干扰,并且开发出一种新的可同时测定水产品中13种磺胺类和甲氧苄啶的方法,方法简便准确,14种药物完全分离,重现性高。To develop a method for determining 13 kinds of sulfonamides and trimethoprim residues of aquatic products by ASE-GPC-HPLC,the shrimp and other aquatic products are extracted by ASE and cleaned up by GPC, collected the liquid and concentrated by nitrogen,then enriched,by 1 mL mobile phase constant volume, the liquid was determined by HPLC and quantified by external standard. The result shows that the 13 kinds of simultaneous and trimethoprim have good linear relationship in the range of 0.01 - 1.00 mg/L and 0.02 - 2.00 mg/L,and the correlation coefficients are all above 0. 999 9. Shrimp spiked with 100,200,400 μg/kg three concentration levels of 13 kinds of sulfonamides and trimethoprim mixed standard solution, the average recovery rates of standard are between 77.9% -98.6%, and RSD is between 0.4% - 13.4%. The study showed that the new method was simple and accurate, and 14 drugs were separated completely.

关 键 词：磺胺类 甲氧苄啶 加速溶剂萃取 凝胶渗透色谱 高效液相色谱 水产品 

分 类 号：TS254.1[轻工技术与工程—水产品加工及贮藏工程]