HPLCMS/MS法检测中华鳖中磺胺类药物残留  

SIMULTANEOUS DETERMINATION OF TWENTY ONE SULFONAMIDE RESIDUES IN TRIONYX SINENSIS BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY

作　　者：张永正[1] 徐晓林 张海琪 方美娟[1] 潘立新[1] 陆红法[1] 

机构地区：[1]浙江海洋学院萧山科技学院,杭州311258 [2]浙江省水产技术推广总站,杭州310012

出　　处：《水生生物学报》2008年第5期669-679,共11页Acta Hydrobiologica Sinica

基　　金：浙江省科技厅重点科研项目基金项目(No.2005C23067)资助

摘　　要：建立了一种液相色谱-电喷雾串联质谱同时测定中华鳖中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1mL流动相溶解,饱和正己烷脱脂净化。采用ZORBAX Ec lipse 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4μg/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75.2%—104%;相对标准偏差为0.16%—9.98%。Sulfonamides are widely used in fisheries for prevention of diseases.With the public＇s increasing concern with the food safety,residues of sulfonamides in fishery products should arouse regards.Improper use or improper withdraw time will lead to the presence of sulfonamide residues in fishery products,which can influence human food security and pollute environment possibly.Many countries have established the maximum allowable residue limits for sulfonamides in fishery products.Therefore,it is necessary to establish the analysis method for the detection of sulfonamides residues in fishery products.A method of simultaneous determination of twenty-one commonly used sulfonamide residues in Trionyx 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 1mL mobile phase and defatted with n-hexane（saturated by acetonitrile）.The 21 analytes were separated on ZORBAX Eclipse XDB-C8 Column with mobile phases containing methanol and 0.2% acetic acid and finally determined by electrospray ionization tandem mass spectrometry（ESI-MS-MS）.A linear gradient eluting program of methanol from 30% to 80%（V /V） was employed at a flow rate of 0.2mL/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 4μg/kg.Recoveries tested by standard addition method were in the range of 75.2%—104%,RSDs were in the range of 0.16%—9.98% at a spiking level from 4μg/kg to 40μg/kg（n=6）.

关 键 词：高效液相色谱-串联质谱 中华鳖 磺胺类药物 检测 

分 类 号：X830.2[环境科学与工程—环境工程]