振荡萃取-超高效液相色谱/质谱法测定土壤中四环素、土霉素及金霉素  

Through Oscillation Extraction Ultra High Performance Liquid Chromatography/Mass Spectrometry,the Determination of Tetracycline,Oxytetracycline and Chloramphenicol in Soil is Accomplished

作　　者：赵佳文 陈美芬 ZHAO Jiawen;CHEN Meifen(At the Jiangxi Province Environmental Monitoring Centre,Nanchang JiangXi 330046,China)

机构地区：[1]江西省生态环境监测中心,江西南昌330046

出　　处：《江西化工》2025年第1期71-75,共5页Jiangxi Chemical Industry

摘　　要：为了高效准确地检测土壤中土霉素、四环素、金霉素的含量,本文提出了一种基于振荡萃取-超高效液相色谱/质谱原理的痕量检测方法。本文通过不同实验条件的对比进行了萃取液保存条件、色谱条件等方法优化,并进行了结果验证,具体实验操作及结果如下。在样品中添加Na2EDTA-Mcllvaine-乙腈提取液后进行振荡离心,上清液通过HLB固相萃取柱进行净化富集。使用Agilent C_(18)色谱柱(2.1 mm×100 mm,1.7μm)进行梯度洗脱,流动相为0.1%甲酸水溶液、0.1%甲酸乙腈溶液,流速为0.2 mL/min,柱温为30℃,进样量为2μL,电喷雾离子源(ESI),正离子模式,毛细管电压为4000 V,干燥气温度为350℃,雾化器压力为35 psi。土霉素、四环素、金霉素的质量浓度与对应色谱峰面积呈良好线性关系,在1.00~500μg/L范围内,检出限分别为0.2μg/kg、0.2μg/kg、0.2μg/kg,相对标准偏差为1.9%~6.4%(n=6),加标回收率为95.7%~100.6%。该方法适用于土壤中土霉素、四环素、金霉素痕量的检测。该方法可用于检测土壤中土霉素、四环素、金霉素的残留量。In order to efficiently and accurately detect the content of oxytetracycline,tetracycline,and aureomycin in soil,this paper proposes a trace detection method based on oscillation extraction ultra-high performance liquid chromatography/mass spectrometry principle.This article optimized the storage and chromatographic conditions of the extraction solution by comparing different experimental conditions,and verified the results.The specific experimental procedures and results are as follows:Mix the Na2EDTA Mcllvaine acetonitrile extract with the sample,shake,then centrifuge the mixture.Afterwards,purify and enhance the supernatant using an HLB solid-phase extraction column.Employ an Agilent C_(18) chromatographic column(2.1 mm×100 mm,1.7μm)with a flow rate of 0.2 mL/min,0.1%formic acid aqueous solution and 0.1%formic acid acetonitrile solution as mobile phases,and gradient elution.Maintain the column temperature at 30℃and inject 2μl of the mixture.The ESI electric spray ion source operates in positive ion mode with a capillary voltage of 4000 V,a dry gas temperature of 350℃,and an atomizer pressure of 35 psi.The mass concentrations of oxytetracycline,tetracycline and aureomycin are between 1.00 and 500μg/L The linear relationship between the g/L range and the corresponding chromatographic peak area is good,with detection limits of 0.2μg/kg,0.2μg/kg,and 0.2μg/kg,the relative standard deviation of the determination results is between 1.9%and 6.4%for concentrations ofμg/kg,with a recovery rate of 95.7%to 100.6%when adding the standard.This particular method is effective in identifying traces of oxytetracycline,tetracycline,and chlortetracycline in soil samples.

关 键 词：四环素类 振荡萃取 土壤 液相色谱串质谱仪 

分 类 号：O657.63[理学—分析化学] X833[理学—化学]