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.
出处
《中国海洋药物》
CAS
CSCD
北大核心
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