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目的:建立了虾中氯霉素、甲砜霉素、氟甲砜霉素三种氯霉素类药物残留的同位素稀释高效液相色谱-串联质谱测定方法。方法:以氘代氯霉素(CAP-d5)为内标,样品用乙腈提取,正己烷脱脂,LC-Si硅胶柱净化,丙酮-正己烷洗(6+4)洗脱后吹氮浓缩。采用Atlantis○R T3质谱柱分离,以乙腈-水-乙酸铵溶液为流动相进行梯度洗脱,以负离子多反应监测模式、同位素内标法定量。结果:方法的检出限和定量限分别为0.03μg/kg、0.10μg/kg;氯霉素、甲砜霉素、氟甲砜霉素回收率分别为82.0%~99.3%、73.5%~85.6%、76.0%~98.5%;相对标准偏差为4.0%-12.5%。应用建立的方法对90份虾样进行分析,其中3份检出氯霉素,含量为1.0μg/kg~4.3μg/kg。结论:本法具有非常高的选择性、灵敏度和准确度,完全能满足虾中痕量氯霉素类药物残留的高灵敏分析。
OBJECTIVE: To establish a method for the determination of three chloramphenicol residues in chloramphenicol, thiamphenicol and florfenicol in shrimp by isotope dilution-high performance liquid chromatography-tandem mass spectrometry. Methods: The deuterated chloramphenicol (CAP-d5) was used as internal standard. The sample was extracted with acetonitrile, defatted with n-hexane, purified with LC-Si silica column and eluted with acetone-n-hexane (6 + 4). The samples were separated on an Atlantis ○ R T3 column and eluted with a mobile phase of acetonitrile-water-ammonium acetate. The mobile phase was quantified by anionic multi-reaction monitoring and isotope internal standard method. Results: The detection limits and the limits of quantitation were 0.03μg / kg and 0.10μg / kg respectively. The recoveries of chloramphenicol, thiamphenicol and florfenicol were 82.0% -99.3% and 73.5% -85.6, respectively %, 76.0% ~ 98.5%; relative standard deviation was 4.0% -12.5%. Ninety batches of shrimp samples were analyzed by using the established method. Among them, three samples were detected with chloramphenicol content of 1.0μg / kg ~ 4.3μg / kg. Conclusion: This method has a very high selectivity, sensitivity and accuracy, fully meet the high sensitivity of trace chloramphenicol residues in shrimp.