首页|液相色谱-串联质谱法测定牛肉中加替沙星残留量的研究

液相色谱-串联质谱法测定牛肉中加替沙星残留量的研究

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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(r2 =0.999);方法检出限和定量限分别为1.0 和2.0 μg/kg;在2.0、4.0、50 μg/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.
Determination of Gatifloxacin Residues in Beef by Liquid Chromatography-tandem Mass Spectrometry
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(r2 =0.999),the limit of detection and limit of quantification was 1.0 and 2.0 μg/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 50.0 μg/kg.This method is fast,accurate and sensitive,can be used for determination of gatifloxacin residues in beef.

liquid chromatography-tandem mass spectrometricbeefgatifloxacinresidues

邵兵、杨修镇、刘霄飞、时川

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山东省畜产品质量安全中心, 济南 250010

液相色谱-串联质谱法 牛肉 加替沙星 残留量

2024

中国兽药杂志
中国兽医药品监察所

中国兽药杂志

CSTPCD
影响因子:0.49
ISSN:1002-1280
年,卷(期):2024.58(4)
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