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环境化学  2015 

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

Keywords: 磺胺类抗生素(SAs),高效液相色谱-串联质谱法(HPLC-MS/MS),蔬菜

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Abstract:

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10mL乙腈(添加2g无水硫酸钠、0.1g乙酸钠、0.1gNa2EDTA)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.

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