超高效液相色谱-串联质谱法快速筛查水产品中氯霉素类药物残留

Rapid Screening of Three Chloramphenicols in Aquatic Products by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱法快速筛查水产品中三种氯霉素类残留的定性定量分析方法。样品经正己烷除脂后用正己烷饱和的乙腈提取,氮气下浓缩至干用流动相复溶,采用电喷雾负离子模式下多反应监测(MRM)模式进行检测,基质匹配标准溶液定量分析。结果表明,在0.5-20 ng/mL的浓度范围内,三种氯霉素具有良好的线性关系,相关系数均大于0.999 8,方法检出限为0.001-0.006μg/kg。在鱼、虾、蟹三种水产品基质中的加标回收率为61.8-103.6%,相对标准偏差(RSD)为2.7-10.9%。该方法简便快速、准确可靠,适用于对大批量水产品样品中氯霉素类残留的快速筛查。

A qualitative and quantitative analysis method was developed for rapid screening of three chloram⁃phenicols in aquatic products by ultra high performance liquid chromatography-tandem mass spectrometry.The samples were degreased with n-hexane and extracted with n-hexane-saturated acetonitrile.The samples were con⁃centrated to dryness under nitrogen and redissolution with mobile phase.The samples were detected by multiple reaction monitoring(MRM)mode under negative ion mode of electrospray,quantitative analysis of matrix match⁃ing standard solution.The results showed that in the concentration range of 0.5-20 ng/mL,the three chloram⁃phenicols had a good linear relationship,the correlation coefficients were higher than 0.9998,and the detection limit of the method was 0.001-0.006μg/kg.The spiked recoveries in the three aquatic product matrices of fish,shrimp,and crab were 61.8-103.6%,and the relative standard deviations(RSDs)were 2.7-10.9%.The method is simple,rapid,accurate and reliable,and is suitable for the rapid screening of chloramphenicos in a large number of aquatic product samples.