摘要
采用超高效液相色谱-串联质谱仪(UPLC-MS/MS)同时快速测定鱼用配合饲料中的氯霉素、甲砜霉素和氟苯尼考3种药物。样品由乙酸乙酯2次提取,经旋蒸浓缩、流动相溶解、正己烷净化后,采用超高效液相色谱C18柱,以5mmol/L乙酸铵溶液-甲醇作流动相梯度洗脱分离,电喷雾负离子多反应监测模式(MRM)检测,内标法定量。氯霉素和氟苯尼考的定量限均为0.30μg/kg,线性范围均为0.20~50.0μg/L;甲砜霉素的定量限为0.5μg/b,线性范围为0.5-50.0μg/L。氯霉素在0.5、1.0、4.0μg/kg和甲砜霉素、氟苯尼考在2.0、10.0、50.0μg/kg的添加水平上的加标回收率为79.8%-102.5%,所有测定结果的日内和日间相对标准偏差(RSD)均小于15%。该方法简便快捷,准确度和精密度高,能够满足鱼用配合饲料中氯霉素类药物同时检测的要求。
A method was developed for simultaneous determination of ehloramphenicol, thiamphenicol and florfenicolresidues in fish formula feed by using ultra - high performance liquid chromatography - tandem mass spectrometry (UPLC -MS/MS). The homogenized samples were extracted twice with ethylacetate and dried by evaporator, redis- solved into 2 mL mobile phase, and then cleaned by n -hexane. The targeted compounds were separated on C18 (2.1 mm ×50mm, 1.7μm)column by using 5 mmol/L ammonium acetate solution -methanol as mobile phase. Multiple reaction monitoring (MRM) with electrespray ionization in positive mode was used for detection. Quantitation limit for chloramphenicol and florfenicol were 0.30 μg/kg with good linearity ranging from 0.20 - 50.0μg/L, and quantita- tion limit for thiamphenicol was O. 50 μg/kg with good linearity ranging from 0.50 - 50.0μg/L. Recoveries spiked in negative samples at the levels of 2.0 -50.0μg/kg were 79.8% - 102.5%. The relative standard deviations(RSD) for all tests were less than 15%. With the advantages of simplicity, rapidity, high accuracy and precision, this meth- od could be suitable for the rapid detection of phenicols residue in fish formula feed.
出处
《中国渔业质量与标准》
2013年第3期44-50,共7页
Chinese Fishery Quality and Standards
基金
浙江省重点科技创新团队项目(2010R50028)
关键词
饲料
氯霉素
超高效液相色谱-串联质谱(UPLC-MS
MS)
fish formula feed
phenicols
uhra -high performance liquid chromatography -tandem mass spectrome-try ( UPLC - MS/MS)