摘要
建立了饲料中氯霉素(CAP)、甲砜霉素(TAP)、氟甲砜霉素(FF)3种抗生素残留量的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。样品经碱化乙酸乙酯提取,蒸发浓缩,提取物经正己烷脱脂,液-液分配净化后,采用电喷雾电离源(ESI)负离子多反应监测(MRM)模式检测,内标法定量。氯霉素、氟甲砜霉素和甲砜霉素的线性范围分别为0.2～10.0、0.2～10.0、1.0～50.0μg/L,相关系数(r2)不低于0.990 0;其检出限分别为0.1、0.1、0.5μg/kg,定量下限分别为0.3、0.3、1.5μg/kg。3种抗生素药物的平均回收率为77%～108%,相对标准偏差(RSD)不大于10.9%。
A method for the determination of three antibiotic drugs,including chloramphenicol（CAP）,thiamphenicol（TAP） and florfenicol（FF） in feed was developed using high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.The target analytes were extracted with basic ethylacetate,and evaporated to dryness.The extracts were defatted with hexane and cleaned up by liquid-liquid partition.Three analytes were detected with electrospray ionization（ESI） in negative mode using multiple reaction monitoring,and quantified by the internal standard method.Under the optimal conditions,the calibration curves of chloramphenicol,florfenicol and thiamphenicol were linear in the ranges of 0.2-10.0,0.2-10.0 μg/L and 1.0-50.0 μg/L,respectively,with correlation coefficients not less than 0.990 0.The limits of detection（LODs） were 0.1,0.1,0.5 μg/kg,and the limits of quantitation（LOQs） were 0.3,0.3,1.5 μg/kg,respectively.The average recoveries ranged from 77% to 108% with RSDs not more than 10.9%.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第1期117-121,共5页
Journal of Instrumental Analysis
基金
江苏出入境检验检疫局科技专项(2009KJ01)
关键词
高效液相色谱-串联质谱
饲料
氯霉素
甲砜霉素
氟甲砜霉素
high performance liquid chromatography - tandem mass spectrometry
feed
chloram-phenicol
thiamphenicol
florfenicol
