摘要
建立了水产品中15种喹诺酮类药物(QNs)残留量的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。以氘代试剂为内标,样品经酸性乙腈萃取后,用正己烷脱脂,旋转蒸发浓缩,采用HPLC-MS/MS选择反应监测(SRM)正离子模式测定,内标法定量。可同时对水产品中的15种QNs进行定性和定量测定。15种QNs的检出限(S/N=3)为1.0μg/kg,定量限(S/N=10)为2.0μg/kg;在10.0～200.0ng/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66%～121%。该法简便快捷,分析成本低,在一定程度上实现了药物残留的快速检测。
A method for simultaneous determination of 15 QNs residues in aquatic products was developed by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. Deuterium substituted reagents were added to the sample before extraction as internal standard. The sample was extracted with acidified acetonitril,cleaned-up with hexane,and concentrated with a rotary evaporator.The mass spectrometer was operated in positive ion mode using select reaction monitoring for qualitative and quantitative analysis of 15 QNs at the same time. The detection limits for 15 QNs were 1.0 μg/kg （S/N=3）,and the quantitation limits were 2.0 μg/kg （S/N=10）. The correlation coeficients of linear calibration curves were over 0.99 within the QNs concentration range 10.0~200.0 ng/mL. The average recoveries for 15 QNs were between 66% and 121%. The method features simple operation,low cost and fast analysis.
出处
《分析科学学报》
CAS
CSCD
北大核心
2010年第4期409-414,共6页
Journal of Analytical Science
基金
国家863计划(No.2008AA100805)
农业部行业专项(Nyhyzx07-046)
基本科研业务费(2007-gy-02)
关键词
高效液相色谱-串联质谱
内标法
水产品
喹诺酮类药物
多残留同时测定
High performance liquid chromatography-tandem mass spectrometry
Internal standard method
Aquatic products
Quinolone
Multi-residue
Simultaneous determination
