液相色谱-串联质谱法测定牛肉中加替沙星残留量的研究  

Determination of Gatifloxacin Residues in Beef by Liquid Chromatography-tandem Mass Spectrometry

作　　者：邵兵 杨修镇 刘霄飞 时川 SHAO Bing;YANG Xiu-zhen;LIU Xiao-fei;SHI Chuan(Shandong Livestock Product Quality and Safety Center,Jinan 250010,China)

机构地区：[1]山东省畜产品质量安全中心,济南250010

出　　处：《中国兽药杂志》2024年第4期62-68,共7页Chinese Journal of Veterinary Drug

摘　　要：建立牛肉中加替沙星残留量检测的液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)方法。牛肉样品经80%(V/V)乙腈溶液提取,Prime HLB固相萃取柱净化。采用0.1%甲酸(V/V)-甲醇溶液和0.1%甲酸(V/V)-水溶液进行梯度洗脱,电喷雾离子源正离子扫描模式(ESI^(+)),多反应监测(MRM),内标法定量。结果表明,加替沙星进样浓度在1~100 ng/mL范围内与峰面积呈良好的线性关系(r^(2)=0.999);方法检出限和定量限分别为1.0和2.0μg/kg;在2.0、4.0、50μg/kg 3个添加水平上,回收率在64.2%~114.6%之间,相对标准偏差为5.5%~9.7%(n=6)。本方法快速、准确、灵敏,适用于牛肉中加替沙星残留量检测。To establish a method for determination of gatifloxacin in beef by liquid chromatography-tandem mass spectrometric(LC-MS/MS),beef samples were extracted with 80%(V/V)acetonitrile solution and then the extracts were purified by the Prime HLB solid phase extraction.The gradient elution was carried out with 0.1%(V/V)formic acid methanol and 0.1%(V/V)formic acid water.Positive ion scanning mode of electric spray ion source(ESI^(+)),multiple reaction monitoring(MRM),internal standard method were applied for quantitative analysis.There was a good linear correlation between the peak areas and the concentrations of gatifloxacin at the range of 1-100 ng/mL(r^(2)=0.999),the limit of detection and limit of quantification was 1.0 and 2.0μg/kg.The recovery rates were 64.2%-114.6%and the relative standard deviations were 5.5%-9.7%(n=6)at the addition levels of 2.0,4.0 and 50.0μg/kg.This method is fast,accurate and sensitive,can be used for determination of gatifloxacin residues in beef.

关 键 词：液相色谱-串联质谱法 牛肉 加替沙星 残留量 

分 类 号：S859.84[农业科学—临床兽医学]