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).