摘要
建立水产品中18种磺胺类药物(SAs)残留量的HPLC-MS/MS测定方法。以氘代试剂为内标,样品经酸化乙腈萃取后,用正己烷脱脂,旋转蒸发浓缩,采用LC-MS-MS选择反应监测(SRM)正离子模式测定,可同时对水产品中的18种SAs进行定性和定量。SAs的检出限(RSN=3)在0.5μg/kg以下,定量限为1.0μg/kg;其中磺胺苯吡唑和磺胺胍检出限(RSN=3)为1.0μg/kg,定量限为2.0μg/kg。在5.0～200.0μg/ml时峰强度与质量浓度的线性关系良好(r>0.99)。方法的平均回收率范围为70%～120%。该法简便快捷,在一定程度上实现了药物残留的快速检测。
The method for simultaneous determination of 18 sulfonamide residues （SAs） in aquatic was developed by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. Deuterium substituted reagents were used as internal standards and added to the sample before extraction. The sample was extracted with acidified acetonitrile, cleaned up with hexane, and concentrated with a rotary evaporator.The mass spectrometer was operated in the positive ion mode using select reaction monitoring for qualitative and quantitative analysis of 18 SAs at the same time. The limits of detection for SAs were 0.5μg/kg （RSN =3） except for sulfaguanidine and sulfaphenazole,which were 1.0 μg/kg, and the limits of quantitation were 1.0 μg/kg, except sulfaguanidine and sulfaphenazole,which were 2.0 μg/kg. The correlation coeficient of linear calibration curve was over 0.99 within the SAs concentration range 5.0-200 μg/ml except for sulfaguanidine and sulfaphenazole.The average recoveries for 18 SAs were 70% to 120%. The method are simple operation, and it make fast analysis come true.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2009年第24期294-298,共5页
Food Science
基金
农业部鲆鲽类行业专项(nyhyzx07-046)
国家"863"计划项目(2008AA100805)
中央级科研院所基本科研经费项目(2007-gy-02)
关键词
高效液相色谱-串联质谱
内标法
水产品
磺胺类药物
多残留
同时测定
high performance liquid chromatography-tandem mass spectrometry
internal standard method
aquatic products
sulfonamide
multi-residue
simultaneous determination
