超声辅助-分散固相萃取/高效液相色谱串联质谱法联用测定鱼肝脏中喹烯酮的残留量  

Determination of Quinocetone Residues in Liver Tissue of Fish by Ultrasonicassisted Extraction Coupled with QuEChERS Extraction and High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：尹怡[1] 李平杰[2] 林晨[3] 刘书贵[1] 朱新平[1] 郑光明[1] 陈昆慈[1] 刘毅辉[1] 宋怿[4] 王群[4] 

机构地区：[1]中国水产科学研究院珠江水产研究所农业部热带亚热带水产种质资源利用与养殖重点实验室农业部水产品质量安全风险评估实验室(广州),广东广州510380 [2]广东药学院药科学院,广东广州510006 [3]中国广州分析测试中心,广东广州510070 [4]中国水产科学研究院,北京100141

出　　处：《分析测试学报》2013年第11期1349-1353,共5页Journal of Instrumental Analysis

基　　金：中国水产科学研究院基本科研业务费专项(2012A1006);广东省水产品质量安全专项资金

摘　　要：建立了快速、准确、灵敏检测鱼肝脏中喹烯酮的超声辅助-分散固相萃取/高效液相色谱-串联质谱(UAE-QuEChERS/HPLC-MS/MS)联用方法。对萃取溶剂、萃取方式与时间、分散吸附剂的种类及质量等条件进行了考察与优化。方法以乙酸乙酯为萃取溶剂,乙二胺-N-丙基硅烷(PSA)与石墨化炭黑(GCB)为固相分散吸附剂,电喷雾正离子(ESI^+)模式电离,多反应监测模式检测,外标法定量。结果表明:在优化实验条件下,方法的线性范围为5~100μg/L,相关系数(r)为0.998 8。方法检出限(LOD,S/N=3)为5μg/kg,定量下限(LOQ,S/N=3)为10μg/kg。采用该方法对杂交鳢的空白肝脏进行检测以及加标回收实验,在10、25、100μg/kg 3个加标水平下,加标回收率为98.6%~110.0%,相对标准偏差(n=3)为5.9%~10.1%。将方法用于杂交鳢体内残留消除规律的研究,发现喹烯酮在杂交鳢体内消除较快,消除半衰期为2.31 h,表明喹烯酮用于杂交鳢的养殖是安全的。A simple,sensitive and accurate method consisted of ultrasound assisted extraction （UAE） coupled with QuEChERS and high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） was developed for the determination of quinocetone （QCT） in liver tissue of fish.The extraction solvent,extraction time and solid sorbent were optimized.The liver tissues were extracted with ethyl acetate,and purified by the mixture of primary secondary amine（PSA） and graphitized carbon blacks（GCB）.The identification of QCT were achieved by using electrospray ionization in positive ion mode （ESI＋） under multiple reaction monitoring（MRM） mode.The analysis of QCT was performed by the external standard method.The calibration curve was linear in the range of 5-100 μg/L with a correlation coefficient of 0.998 8.The limit of detection（LOD,S/N=3） was 5 μg/kg and the limit of quantitation（LOQ,S/N=10） was 10 μg/kg.The method was applied in the determination of QCT in the hybrid snakehead liver tissues,and the recoveries at three spiked levels of 10,25,100 μg/kg ranged from 98.6% to 110.0% with relative standard deviations （RSDs,n=3） of 5.9%-10.1%.The proposed method was applied in the final residue detection after feeding Hybrid Snakehead with feed containing 75 mg/kg QCT for 60 consecutive days.The result showed that QCT was depleted quite fast in hybrid snakehead,and the elimination half life time of snakehead was 2.31 h.Therefore,it could be concluded that QCT was safe in feeding Hybrid Snakehead.

关 键 词：超声辅助萃取 固相分散萃取 高效液相色谱-串联质谱 肝脏 喹烯酮 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]