生态环境部南京环境科学研究所,国家环境保护农药环境评价与污染控制重点实验室,江苏 南京 210042
孔德洋,研究员,研究方向:农药环境行为研究,E-mail:kdy@nies.org
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曹莉,李菊颖,余佳等.环境介质中噻酮磺隆及其代谢产物的液相色谱-串联质谱测定方法研究[J].分析测试学报,2023,42(07):849-855.
CAO Li,LI Ju-ying,YU Jia,et al.Determination of Thiencarbazone-methyl and Its Metabolites in Different Environmental Matrixes by Liquid Chromatography- Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(07):849-855.
曹莉,李菊颖,余佳等.环境介质中噻酮磺隆及其代谢产物的液相色谱-串联质谱测定方法研究[J].分析测试学报,2023,42(07):849-855. DOI: 10.19969/j.fxcsxb.23020702.
CAO Li,LI Ju-ying,YU Jia,et al.Determination of Thiencarbazone-methyl and Its Metabolites in Different Environmental Matrixes by Liquid Chromatography- Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(07):849-855. DOI: 10.19969/j.fxcsxb.23020702.
建立了水、土壤和沉积物中噻酮磺隆及其代谢产物噻酮酸(M01)、噻吩酸(M03)、噻酮磺胺(M15)的液相色谱-串联质谱(LC-MS/MS)分析方法。水样酸化后采用HLB柱进行固相萃取,土壤和沉积物经酸化乙腈提取、N-丙基乙二胺(PSA)净化后,利用Agilent Poroshell 120EC-C,18,(2.1 mm × 75 mm,2.7 μm)色谱柱以乙腈与水为流动相进行梯度洗脱分离,电喷雾离子源、多反应离子监测模式(MRM)下进行负离子检测,外标法定量。噻酮磺隆及3种代谢产物在0.001 ~ 0.1 mg/L范围内线性良好(,r,2,>, 0.995)。在0.1、1、10 µg/L加标水平下,水样中4种目标物的平均回收率为75.5% ~ 104%,相对标准偏差(RSD,,n, = 5)为1.4% ~ 8.6%;在0.5、5、50 µg/kg加标水平下,土壤和沉积物中4种目标物的平均回收率为75.4% ~ 105%,RSD为1.5% ~ 9.7%;水样中定量下限(LOQ)为0.1 µg/L,土壤和沉积物中LOQ为0.5 µg/kg。该方法灵敏度高、重现性好,适用于环境介质中噻酮磺隆及其代谢产物的测定。
A liquid chromatography-tandem mass spectrometry(LC-MS/MS) was established for the simultaneous determination of thiencarbazone-methyl and its metabolites including BYH18636-carboxylic acid(M01),BYH18636-sulfonamide-carboxylic acid(M03),BYH18636-sulfonamide(M15) in water,soil and sediments.Water samples were firstly acidated by formic acid,then extracted with HLB solid phase extraction(SPE) cartridge,while the soil and sediments samples were firstly extracted with acidated acetonitrile and cleaned up with primary secondary amine(PSA) cartridge,then detected by LC-MS/MS.The separation was carried out on an Agilent Poroshell 120EC-C,18,(2.1 mm × 75 mm,2.7 μm) column by gradient elution with acetonitrile and water as the mobile phases.The detection was carried out with electrospray ion source in negative ion mode under multi-reaction monitoring(MRM) mode.External standard method was applied to obtain the matrix-matched calibration curve for quantification.Results showed that there were good linear relationships for thiencarbazone-methyl and its metabolites in the range of 0.001-0.1 mg/L,with their correlation coefficients(,r,2,) more than 0.995.The average recoveries for water samples at three spiked levels of 0.1,1 and 10 µg/L ranged from 75.5% to 104%,with relative standard deviations(RSDs,,n ,= 5) of 1.4%-8.6%,while the recoveries for soil and sediment samples at three spiked levels of 0.5,5 and 50 µg/kg ranged from 75.4% to 105%,with RSDs of 1.5%-9.7%.The quantification limit of four analytes was 0.1 µg/L in water,while 0.5 µg/kg in soil and sediments.With high sensitivity,accuracy and good repeatability,this method is suitable for the simultaneous determination of thiencarbazone-methyl and its metabolites in water,soil and sediments.
噻酮磺隆代谢产物液相色谱-串联质谱固相萃取
thiencarbazone-methylmetabolitesliquid chromatography-mass spectrometrysolid phase extraction
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