【摘要】 建立了一种液相色谱-电喷雾串联质谱同时测定中华绒螯蟹中21种磺胺类药物残留的方法。均质样品先后用乙腈、二氯甲烷提取,合并提取液,取部分提取液经氮吹浓缩。残渣用1 mL流动相溶解,饱和正己烷脱脂净化。采用ZOR-BAX Eclipse XDB-C8色谱柱,以含0.2%乙酸的水溶液和甲醇(7:3)为流动相,梯度洗脱,在电喷雾-多反应监测离子模式下,进行定量定性分析。方法的定量限为5μg/kg;以标准加入法计算回收率,在4～40μg/kg添加范围内,平均回收率为71.8%～106%;相对标准偏差为0.44%～10.1%。更多还原

【Abstract】 The method of simultaneous determination of twenty commonly used sulfonamide residues in Eriocheir sinensis by high performance liquid chromatography-electro spray tandem mass spectrometry(HPLC/ MS/MS) is described.Sulfonamide residues were extracted from homogenized tissue with acetonitrile and dichloromethane.A part of the extract was taken and then dried by nitrogen.The residues were dissolved into 1 mL mobile phase and defatted with n-hexane(saturated by acetonitrile).The 21 analytes were separated on ZORBAX Eclipse XDB-C8 Column with mobile phases containingmethanol and 0.2% acetic acid and finally determined by electrospray ionization tandem mass spectrometry(ESI-MS-MS).A linear gradient eluting pro-gram of methanol from 30% to 80%(V/V) was employed at a flow rate of 0.2 mL/min in 35 minutes.Analytes confirmation were performed using multiple reaction monitoring(MRM) with one precursorion and two product ions as identifiers.The quantitative limit of method was 5 μg/kg.Recoveries tested by standard addition method were in the range of 71.8%-106%,RSDs were in the range of 0.44%-10.1% at a spiking level from 4 μg/kg to 40 μg/kg(n= 6).更多还原