首页|超高效液相色谱-串联质谱法同时测定土壤及沉积物中81种农药和抗生素

超高效液相色谱-串联质谱法同时测定土壤及沉积物中81种农药和抗生素

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建立超高效液相色谱-串联质谱法同时测定土壤和海洋沉积物中53种农药和28种抗生素残留.样品分别经酸化乙腈(含0.5%甲酸)和Mcllvaine-Na2EDTA缓冲液(pH 5.0)提取后,利用PRiME HLB固相萃取柱净化,通过ACQUITY UPLC BEH C18柱分离,在优化的仪器工作条件下测定,用外标法定量.81种化合物的质量浓度在1.0~100.0 μg/L范围内与色谱峰面积线性关系良好,相关系数均大于0.99,方法定量限为5.0~10.0 μg/kg.81种化合物的加标平均回收率为66.5%~115.5%,测定结果的相对标准偏差为0.3%~15.2%(n=6).土霉素等4种化合物的基质效应为55.2%~105.2%,基质增强效应较强,强力霉素等5种化合物为中等基质效应,其他化合物均为弱基质效应.该方法可用于同时测定土壤及沉积物中81种农药和抗生素残留.
Simultaneous determination of 81 pesticide and antibiotic in soil and sediment by ultra-high performance liquid chromatography-tandem mass spectrometry
A method for simultaneous determination of 53 pesticides and 28 antibiotics residues in soil and marine sediments by ultra-high performance liquid chromatography-tandem mass spectrometry was established.Samples were extracted with acetonitrile solution containing 5.0%formic acid and Mcllvaine-Na2EDTA buffer solution(pH 5.0),purified with PRiME HLB solid-phase extraction column and separated using ACQUITY UPLC BEH C18 column.External standard method was used to the quantitative analysis under the optimized instrument operating conditions.The mass concentration of 81 compounds had a good linear relationship with the chromatographic peak area in the range of 1.0-100.0 μg/L,the correlation coefficients were all more than 0.99.The quantification limits of the method were 5.0-10.0 μg/kg.The average recoveries of 81 compounds were 66.5%-115.5%,and the relative standard deviations of determination results were 0.3%-15.2%(n=6).The matrix effects of 4 compounds,including oxytetracycline were 55.2%-105.2%,exhibited strong matrix enhancement effects,5 compounds,including doxycycline showed medium matrix effects,while the others showed weak matrix effects.The method can be used to simultaneously determine 81 pesticides and antibiotics residues in soil and sediment.

ultra-high performance liquid chromatography-tandem mass spectrometrysoilsedimentpesticidesantibiotics

许炳雯

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大连市检验检测认证技术服务中心,国家市场监督管理总局技术创新中心(食用农产品安全快速检测与追溯),辽宁 大连 116037

超高效液相色谱-串联质谱法 土壤 沉积物 农药 抗生素

2025

化学分析计量
中国兵器工业集团第五三研究所(国防科技工业应用化学一级计量站)

化学分析计量

影响因子:0.444
ISSN:1008-6145
年,卷(期):2025.34(1)