固相萃取-高效液相色谱-串联质谱法同时测定蔬菜中8种磺胺类抗生素  

Simultaneous determination of eight sulfonamide antibiotics in vegetables using solid phase extraction and high performance liquid chromatography coupled with mass spectrometry

作　　者：吴小莲[1,2] 包艳萍[1] 向垒[1] 严青云[1] 姜元能[1] 李彦文[1,2] 黄献培[1,2] 莫测辉[1] 

机构地区：[1]暨南大学环境工程系,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 [2]暨南大学水生生物研究所,广州516032

出　　处：《环境化学》2013年第6期1038-1044,共7页Environmental Chemistry

基　　金：国家自然科学基金项目(41173101);广东省自然科学基金重点项目(20110200003196);广东高校高层次人才项目资助

摘　　要：建立了固相萃取-高效液相色谱-串联质谱同时测定蔬菜中8种磺胺类抗生素(SAs)的分析方法.以10 mL乙腈(添加2 g无水硫酸钠、0.1 g乙酸钠、0.1 g Na2EDTA)进行提取,HLB柱净化富集.采用RESTEKPinnacleⅡC18色谱柱,以水(含0.1%甲酸)和乙腈(含0.1%甲酸)为初始流动相进行梯度洗脱.在电喷雾-多反应检测离子模式下,进行定性定量分析.SMZ的方法定量限为0.2μg·kg-1,其它7种化合物的定量限均为0.1μg·kg-1.不同加标浓度(5—100μg·kg-1)下8种SAs的回收率大部分约在70%以上,相对标准偏差(RSD)多数小于10%,表明该方法能够满足实际样品的分析要求.利用该方法对某无公害蔬菜基地进行分析,蔬菜中检出3种以上磺胺类抗生素,含量在0.20—17.43μg·kg-1(干重)之间,总含量在2.42—27.60μg·kg-1之间.An analytical method for the simultaneous determination of eight sulfonamide antibiotics（sulfadimethoxine,sulfpyride,sulfamethazine,sulfathiazole,sulfamerazine,sulfamethoxazole,sulfameter and sulfadiazine）in vegetables was presented using solid phase extraction and high performance liquid chromatography coupled with mass spectrometry.Vegetable samples were extracted by acetonitrile（containing 2 g anhydrous sodium sulfate,0.1 g sodium acetate and 0.1 g disodium ethylenediamine tetraacetate）,then purified and enriched by the HLB column.The sulfonamide antibiotics were separated on RESTEK Pinnacle Ⅱ C18 column with mobile phase containing 0.1% acetic acid and acetonitrile（0.1% acetic acid） and then determined by electrospray ionization mass spectrometry（ESI-MS）.The quantitative limits of method were 0.2 μg·kg-1 for SMZ and 0.1 μg·kg-1 for the other seven analytes.Recoveries were mostly above 70% and relative standard deviation（RSD） was mostly under 10% at various spiking levels The method was successfully applied to test sulfonamides in vegetable samples with total content from 2.42 μg·kg-1 to 27.60 μg·kg-1.

关 键 词：磺胺类抗生素(SAs) 高效液相色谱-串联质谱法(HPLC-MS MS) 蔬菜 

分 类 号：S481.8[农业科学—农药学]