高效液相色谱串联质谱法同时测定饲料中4种硝基呋喃类抗生素

摘要

建立了同时测定配合饲料中呋喃唑酮、呋喃它酮、呋喃西林、呋喃妥因的高效液相色谱串联质谱(HPLC-MS/MS)分析方法.样品粉碎后经乙腈提取,在40℃下氮气吹干,残渣用正己烷脱色脱脂,经中性氧化铝小柱净化,采用Sunfire C18柱(150 mm ×2.1 mm,5.μm)分离,流动相为甲醇和0.05％乙酸铵溶液,梯度洗脱,在MRM正负切换采集模式下进行测定,外标法定量,其中呋喃西林与呋喃妥因采用负离子扫描方式,呋喃它酮与呋喃唑酮采用正离子扫描方式.呋喃唑酮和呋喃妥因的检出限(LOD)为2.0 μg/kg,定量下限(LOQ)为5.0μg/kg,呋喃它酮和呋喃西林的检出限(LOD)为3.0 μg/kg,定量下限(LOQ)为10.0 μg/kg,4种药物在5.0～ 100.0μg/L范围内线性关系均良好(r＞0.99).以罗非鱼饲料进行加标回收实验,测得4种硝基呋喃原药的回收率为78％～107％,相对标准偏差均小于12％.该方法快速、准确,可用于配合饲料中4种硝基呋喃原药的同时测定.%A method was developed for the determination of furazolidone (FZD),furaltadone (FTD),furacilin (NFZ)and nitrofurantoin(NFT) residues in feedstuff by isotope dillution high performance liquid chromatography-tandem mass spectrometry.After homogenization,samples were extracted with acetonitrile.After centrifugation,the extract was evaporated to dryness with nitrogen at 40℃,and redissolved with acetonitrile-0.05％ ammonium acetate solution.The solution was defatted with hexane and cleaned up with neutral alumina solid phase extraction cartridge.The targeted compounds were seperated on a Sunfire C18 (150 mm × 2.1 mm,5 μm) column by using methanol-0.05％ ammonium acetate as mobile phase,and detected with electrospray ionization (ESI) under positive and negative switching scan mode,in which negative scan mode was used for NFZ and NFT,respectively,and positive scan mode was used for FZD and FTD.The detection limits were 2.0 μg/kg for FZD and NFT and 3.0 μg/kg for FTD and NFZ,respectively.The quantitation limits were 5.0 μg/ L for FZD and NFT,and 10.0 μg/kg for FTD and NFZ,respectively.The linear ranges of the target compounds ranged from 5.0 μg/L to 100.0 μg/L with correlation coefficients greater than 0.99.The recoveries of four compounds in spiked feed for tilapia were in the range of 78％-107％ with relative standard deviations(RSDs) less than 12％.The method is rapid and accurate,and is suitable for the detection of four nitrofuran drugs in feedstuff.