固相萃取-高效液相色谱法分析蔬菜中6种磺胺类抗生素  

DETERMINATION OF SIX SULFONAMIDE ANTIBIOTICS IN VEGETABLES BY SOLID PHASE EXTRACTION AND HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

作　　者：包艳萍[1,2] 李彦文[1,2] 莫测辉[1,2] 姚圆[1,2] 邰义萍[1,2] 吴小莲[1,2] 张艳[1,2] 

机构地区：[1]暨南大学环境工程系,广州510632 [2]广东省高校水土环境毒害性污染物防治与生物修复重点实验室,广州510632

出　　处：《环境化学》2010年第3期513-518,共6页Environmental Chemistry

基　　金：国家自然科学基金项目(30671208;40773062);广东省自然科学基金重点项目(07117909);广东省科技计划项目(2005B20801002;2006B20601003);东莞市科技计划项目(2007108101110);惠州市科技计划项目(2009B10001009)

摘　　要：建立了固相萃取-高效液相色谱同时测定蔬菜中6种磺胺类抗生素的分析方法.以每克蔬菜(干样)加5ml乙腈(添加2g无水硫酸钠、0.1g乙酸钠、0.1gNa2EDTA)超声提取25min,采用正己烷液-液萃取去脂,C18柱净化富集.以磷酸(0.01mol.l-1,pH2.5)∶乙腈=80∶20(V∶V)溶液作为流动相,检测波长为270nm.蔬菜样品中6种磺胺类抗生素的回收率为50.8%—98.9%,定量限为21.9—72.8μg.kg-1.利用该方法对不同蔬菜样品进行了分析,6种磺胺类抗生素均不同程度被检出,总含量在0.38—2.24mg·kg-1(鲜重)之间.In this paper a new analytical methodology for the simultaneous analysis of six sulfonamides in vegetables using high performance liquid chromatography（HPLC）with solid-phase extraction was presented.Vegetable samples were extracted by acetonitrile（adding 2g anhydrous sodium sulfate,0.1g sodium acetate and 0.1g disodium ethylenediamine tetraacetate）,defatted by a double liquid liquid partition with n-hexane,dried in a rotary evaporator,then purified and enriched by the C18 solid phase extraction column.Using acetonitrile and 0.01mol·l-1 phosphoric acid（pH=2.5 with triethylamine）as the mobile phase,270nm as detection wavelength,the recoveries rate were 50.84%—98.91% and the detection limits for six sulfonamides in vegetables were obtained from 21.86 to 72.78 g·kg-1.The method was successfully applied to determine six sulfonamides in various vegetable samples with the total contents of 0.3801—2.2367 mg·kg-1（FW）.

关 键 词：磺胺类抗生素 高效液相色谱 蔬菜 

分 类 号：S481.8[农业科学—农药学]