超高效液相色谱-质谱法测定海洋药用生物中氯霉素残留量  

Determination of chloramphenicol residue in marine drug organisms by UPLC MS/MS with Internal Standard Method

作　　者：陈安珍 杨钊 奚玮 吴爱英 

机构地区：[1]青岛市药品检验所,山东青岛266071

出　　处：《中国海洋药物》2013年第3期67-70,共4页Chinese Journal of Marine Drugs

基　　金：国家高技术发展计划(2008AA100805)资助

摘　　要：目的建立测定海洋药用生物中氯霉素残留的超高效液相色谱-串联质谱方法。方法样品采用乙酸乙酯萃取,氯化钠溶液去蛋白,正己烷去油脂,经液相色谱分离,串联四极杆质谱多反应监测(MRM)模式检测,内标法定量。结果氯霉素的线性范围为0.5～10.0μg.L-1,相关系数为0.995,检测限为0.03μg.kg-1,定量限为0.1μg.kg-1。加标回收率为88.1%～96.8%,RSD为3.3%～4.9%。结论该方法前处理简单、灵敏度和准确度高,适合对海洋药用生物中氯霉素残留的检测。Objective To develop a UPLC-MS/MS method for determination of chloramphenicol residue in marine drug organisms. Methods Samples were extracted with ethyl acetate, removed protein with sodi- um chloride and defatted with hexane. The analytes were separated by UPLC and detected by multi-re- actions monitoring （MRM） technology of tandem mass spectrometry with electrospray ionization source. Results The calibration curve of chloramphenicol showed good linearity in the range of 0. 5 10. 0 μg· L-1 , and correlation coefficient was 0. 995. The limits of detection and quantification in sam- ples were 0.03 and 0. 1μg· kg-1 respectively. The average recoveries ranged from 88. 1%--96.8% with RSD 3.3% to 4. 9%. Conclusion The method is simple, sensitive and accurate. It is suitable for the determination of chloramphenicol residue in marine drug organisms.

关 键 词：超高效液相色谱-串联质谱 海洋药用生物 氯霉素 多反应监测 

分 类 号：R931[医药卫生—生药学]