高效液相色谱串联质谱法同时测定饲料中氯霉素、甲砜霉素与氟甲砜霉素残留  

Simultaneous Determination of Chloramphenicol,Thiamphenicol and Florfenicol Residues in Feedstuff by Isotope Dillution High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李红权 孙良娟 伍志强 黄武 周永奇 梁庭瑜 

机构地区：[1]湛江出入境检验检疫局检验检疫技术中心,广东湛江524001

出　　处：《分析测试学报》2012年第11期1396-1400,共5页Journal of Instrumental Analysis

摘　　要：以D5-氯霉素为内标,建立了高效液相色谱-电喷雾串联质谱测定饲料预混料、配合饲料中氯霉素、甲砜霉素与氟甲砜霉素含量的方法。样品磨碎后,采用乙酸乙酯提取,离心后上清液于45℃下氮气吹干,溶解残渣并用正己烷液液萃取净化处理,经C18固相萃取净化后,通过Agilent Eclipse C18(150 mm×4.6 mm,5μm)色谱柱以甲醇-0.1%甲酸作流动相梯度洗脱分离,采用电喷雾电离(ESI)、多反应监测(MRM)负离子扫描方式进行定性与定量分析。方法的检出限(LOD)为0.5μg/L,定量下限(LOQ)为1.0μg/L,待测物与内标物定量离子的峰面积比值与待测物的质量浓度在0.5～10.0μg/L范围内呈良好线性关系,相关系数(r2)不低于0.999 0。在0.5～2.0μg/kg范围内,3个水平的加标回收率为78%～107%,相对标准偏差(RSDs,n=6)均小于10%。A method was developed for the determination of chloramphenicol, thiamphenicol and florfenicol residues in feedstuff by isotope dillution high performance liquid chromatography - tandem mass spectrometry. After homogenization, the samples were extracted with ethyl acetate. After centrifugation, the extract was evaporated to dryness with nitrogen at 45 ℃, and redissolved with 4 mL ultrapure water. The solution was defatted with hexane and cleaned up by C18 solid phase extraction cartridge. The targeted compounds were seperated on an Agilent Eclipse C18 （150 mm ×4. 6 mm, 5 μm） column by using methanol-0. 1% formic acid as mobile phase. Identification and detection were achieved by electrospray ionization（ESI） under negative mode using multiple reaction monitoring （MRM） mode. The detection limits for the target compounds were all 0. 5 μg/L and the quantitation limits were all 1.0 μg/L. The linear range of the target compounds ranged from 0. 5 μg/L to 10. 0 μg/L with correlation coefficients not less than 0. 999 0. Recoveries of three compounds were in the range of 78% - 107% at the spiked level of 0. 5 -2. 0 μg/kg, with relative standard deviations（RSDs） less than 10%.

关 键 词：同位素内标 高效液相色谱-电喷雾串联质谱法 氯霉素 甲砜霉素 氟甲砜霉素 饲料 

分 类 号：O657.72[理学—分析化学] S859.796[理学—化学]