离子液体单滴微萃取-高效液相色谱法检测肉中的磺胺类药物  

Ionic liquid-based single drop microextraction combined with high performance liquid chromatography for the determination of sulfonamides in meat

作　　者：王庚南[1] 张会彩[1] 刘静[1] 张磊[1] 王建平[1] 

机构地区：[1]河北农业大学动物医学院,河北保定071000

出　　处：《畜牧与兽医》2016年第3期5-10,共6页Animal Husbandry & Veterinary Medicine

基　　金：河北省自然科学基金(C2012204004)资助

摘　　要：建立一种离子液体单滴微萃取法结合高效液相色谱法对肌肉组织中的磺胺类药物进行提取检测。对离子液体及用量、盐析作用、p H值、振荡频率、提取时间等参数进行优化,结果显示：肉组织以乙腈提取,提取液蒸至近干后用蒸馏水稀释到15 m L,调节p H为4.0,添加36%（w/v）的Na Cl,以8μL的1-己基-3-甲基咪唑六氟磷酸盐为萃取剂,调节振荡频率为700 r/min,提取20 min。在最佳的条件下,该法对6种磺胺类药物具有8～29倍的富集倍数,检测限范围为0.5～1.0 ng/g,在肉组织中的添加回收率为70.6%～95.1%。该方法可用于肌肉组织中磺胺类药物残留的检测。The objective of the present study was to develop an ionic liquid based single drop microextraction method for extraction of the residual sulfonamide drugs in meat followed by determination with high performance liquid chromatography. Several important parameters（ ionic liquid and its volume,stirring rate,extraction time,p H and salt addition） that possibly influenced the extraction performance were optimized. Meat samples were extracted with acetonitrile,and the acetonitrile extract was evaporated to nearly dry. The residue extracts were diluted with water to 15 m L（ adjusting p H to 4. 0 and adding 36%（ w / v） Na Cl）,and then a drop of 8 μL 1- hexyl- 3- methylimidazolium hexafluorophosphate was suspended in the solution for 20 min at stirring rate of 700 rpm to accomplish the procedure. Under the optimal conditions,this method showed different enrichment factors（ 8-29 folds） for six sulfonamides（ sulfadiazine,sulfadimidine,sulfadimethoxine,sulfamethoxypyridazine,sulfamonomethoxine,sulfamethoxazole）. The limits of detection of the six sulfonamides were in the range of 0. 5-1. 0 ng / g,and their recoveries from the fortified meat samples were in the range of 70. 6%-95. 1%. It suggests that this method can be used as a sensitive and accurate tool to determine the residues of the six sulfonamides in meat.

关 键 词：离子液体 单滴微萃取 高效液相色谱法 磺胺类药物 肉 

分 类 号：S852.1[农业科学—基础兽医学]