食品科学 ›› 2017, Vol. 38 ›› Issue (24): 241-246.doi: 10.7506/spkx1002-6630-201724039

• 安全检测 • 上一篇    下一篇

基于通过型固相萃取-高效液相色谱-串联质谱法同时测定水产品中的氯霉素和红霉素

柯庆青,李诗言,周凡,郑重莺,贝亦江,王鼎南,王扬   

  1. (浙江省水产质量检测中心,浙江?杭州 310023)
  • 出版日期:2017-12-25 发布日期:2017-12-07
  • 基金资助:
    浙江省2013年农业标准化研究项目

Simultaneous Determination of Chloramphenicol and Erythromycin Residues in Aquatic Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Oasis PRiME HLB Solid Phase Extraction Cleanup

KE Qingqing, LI Shiyan, ZHOU Fan, ZHENG Chongying, BEI Yijiang, WANG Dingnan, WANG Yang   

  1. (Aquatic Products Quality Inspection Center of Zhejiang Province, Hangzhou 310023, China)
  • Online:2017-12-25 Published:2017-12-07

摘要: 建立通过型固相萃取-高效液相色谱-串联质谱同时快速测定水产品中氯霉素和红霉素的分析方法。样品通过乙腈提取,Oasis PRiME HLB小柱一步法净化,采用高效液相色谱-串联质谱仪多反应监测扫描模式检测和同位素内标定量。检测水产品中的氯霉素和红霉素定量限分别为0.1?μg/kg和0.5?μg/kg。不同水产品(鱼、虾和蟹)在3?个添加水平的平均回收率在86.7%~102.6%之间,相对标准偏差小于5%(n=6)。本方法简单易行、灵敏度较高,在日常检测方面存在一定优势。

关键词: 固相萃取, 高效液相色谱-串联质谱, 水产品, 氯霉素, 红霉素

Abstract: A rapid method was developed for the simultaneous determination of chloramphenicol and erythromycin residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry with solid phase extraction (SPE). Samples were extracted with acetonitrile and the extract was then purified by an Oasis PRiME HLB SPE cartridge. The analytes were detected in the multi-reaction monitoring (MRM) mode and quantified by the isotope internal standard method. The limits of quantification (LOQ) for chloramphenicol and erythromycin were 0.1 and 0.5 μg/kg, respectively. The average recoveries of the 2 analytes ranged from 86.7% to 102.6% with relative standard deviations of less than 5% in aquatic products (fish, shrimp and crab) at three spiked levels (n = 6). This proposed method was advantageous in routine detection of antibiotic residues in aquatic products for its simplicity and high sensibility.

Key words: solid phase extraction, high performance liquid chromatography-tandem mass spectrometry, aquatic products, chloramphenicol, erythromycin

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