分析测试学报2017，Vol.36Issue(8)：1029-1032,1037,5.DOI:10.3969/j.issn.1004-4957.2017.08.014
高效液相色谱-串联质谱法测定蜂胶原胶中氯霉素的残留量
Determination of Chloramphenicol in Propolis by High Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A method was developed for the determination of chloramphenicol in propolis by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).The flavonoid was removed with NaOH after the dissolution of the sample with methyl tert-butyl ether(MTBE).The solubility of chloramphenicol in MTBE was decreased with n-hexane,and then chloramphenicol was extracted with sodium acetate buffer.After the extraction was transferred to alkaline solution,ethyl acetate was used to extract chloramphenicol.The supernatant was evaporated,and re-dissolved with water for detection.The separation of chloramphenicol was performed on an Atlantis T3 column with methanol and water(65 ∶ 35,by volume) as mobile phases,and the detection of chloramphenicol was carried out by tandem mass spectrometry in negative electrospray ionization (ESI-) and multiple reaction monitoring(MRM) mode.The quantification was performed by the internal standard method.The calibration curve showed a good linearity in the range of 0.1-5.0 μg/L.The limits of quantitation(S/N ≥ 10) were 0.3 μg/kg.The recoveries at three spiked levels were in the range of 97.3％-103％ with relative standard deviations of 4.8％-6.4％.With the advantages of sensitivity,strong anti-interference capability,good recovery and repeatability,the method was suitable for the monitoring of veterinary residue analysis关键词
蜂胶原胶/氯霉素/高效液相色谱-串联质谱法(HPLC-MS/MS)Key words
propolis/chloramphenicol/high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)分类
数理科学引用本文复制引用
邵琳智,谢敏玲,林峰..高效液相色谱-串联质谱法测定蜂胶原胶中氯霉素的残留量[J].分析测试学报,2017,36(8):1029-1032,1037,5.基金项目
广东省省级科技计划项目(2015A030401075) （2015A030401075）
