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高效液相色谱-串联质谱法测定肠衣中17种磺胺类药物残留量 被引量:12

Determination of 17 sulfonamide residues in casing by liquid chromatography-tandem mass spectrometry
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摘要 建立了一种以13C6-磺胺二甲基嘧啶为内标快速测定肠衣中17种磺胺类药物残留量的方法.样品经过V(乙腈)∶V(乙酸乙酯)=1∶1 混合溶剂提取后,离心,上清液在旋转蒸发仪上蒸发至干,体积分数30%甲醇溶液定容,正己烷除去脂肪,经过滤膜后,进高效液相色谱-串联四极杆质谱进行分析,内标法定量.方法的回收率在80%~100%之间,相对标准偏差在15.4%以下,定量限为1.0 μg/kg(磺胺脒为2.0 μg/kg),检出限在0.4 μg/kg以下(磺胺脒为1.0 μg/kg).方法适合于大批量样品的快速检测. A rapid method of determining 17 sulfonamides residues by using the 13^C6-sulfamethazine as an internal standard in the casing was studied by liquid chromatography-tandem mass spectrometry. Samples were extracted with 1 : 1 acetonitrile and ethyl acetate followed by centrifuging. Then the supematant was evaporated on a rotary evaporator until dry. And 1.0 mL of solution comprised of 30: 70 methanol and pure water was added into the bottle to dissolve the matters of interest and 0.5 mL of hexane was added to remove fat. After filtration with 0.45 /an membrane, the samples were analyzed by high performance liquid chromatography and tandem mass spectrometer. The recoveies concentrated in 80% - 100%, the RSD was below 15.4%, the limit of quantitation was 1.0 μg/kg except Sulfaguanidine, which was 2.0 μg/kg, and the limit of detection was below 0.4 μg/kg (with the exception of Sulfaguanidine which was 1.0 μg/kg).
出处 《分析试验室》 CAS CSCD 北大核心 2007年第5期96-99,共4页 Chinese Journal of Analysis Laboratory
基金 江苏出入境检验检疫局科技项目(2005KJ16)
关键词 磺胺类药物 肠衣 液相色谱-质谱联用 多残留 Sulfonamides Casing Liquid chromatography-tandem mass spectrometry Multi-residue
作者简介 吴宗贤(1981-),男,硕士研究生
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