Determination of Quinocetone Residues in Liver Tissue of Fish by Ultrasonic assisted Extraction Coupled with QuEChERS Extraction and High Performance Liquid Chromatography Tandem Mass Spectrometry
  
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DOI:10.3969/j.issn.1004-4957.年份.月份
KeyWord:ultrasound-assisted extraction(UAE)  QuEChERS  HPLC-MS/MS  liver tissue  quinocetone(QCT)
  
AuthorInstitution
尹怡,李平杰,林晨,刘书贵,朱新平,郑光明,陈昆慈,刘毅辉,宋怿,王群 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);2.广东药学院药科学院;3.中国广州分析测试中心;4.中国水产科学研究院
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Abstract:
      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.
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