1.西北师范大学 地理与环境科学学院,甘肃 兰州 730070
2.甘肃省绿洲资源环境与 可持续发展重点实验室,甘肃 兰州 730070
瞿德业,博士,副教授,研究方向:土壤环境,E-mail:qudeye@nwnu.edu.cn
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瞿德业,王彩虹,陈静等.溶剂诱导萃取/UPLC-MS/MS法检测农田土壤中20种除草剂[J].分析测试学报,2023,42(12):1631-1638.
QU De-ye,WANG Cai-hong,CHEN Jing,et al.Determination of Herbicides in Agricultural Soils by Solvent Induced Extraction Coupled with UPLC-MS/MS[J].Journal of Instrumental Analysis,2023,42(12):1631-1638.
瞿德业,王彩虹,陈静等.溶剂诱导萃取/UPLC-MS/MS法检测农田土壤中20种除草剂[J].分析测试学报,2023,42(12):1631-1638. DOI: 10.19969/j.fxcsxb.23072101.
QU De-ye,WANG Cai-hong,CHEN Jing,et al.Determination of Herbicides in Agricultural Soils by Solvent Induced Extraction Coupled with UPLC-MS/MS[J].Journal of Instrumental Analysis,2023,42(12):1631-1638. DOI: 10.19969/j.fxcsxb.23072101.
采用优化的溶剂诱导萃取前处理方法联合超高效液相色谱-串联质谱(UPLC-MS/MS),建立了同时快速测定土壤中20种除草剂的方法。采用1.5 mL二氯甲烷为萃取剂,5 mL乙腈为提取剂,涡旋时间8 min进行提取,以ZORBAX Eclipse Plus C,18,色谱柱(100 mm×2.1 mm,1.8 μm)进行分离,0.1%甲酸水和乙腈为流动相,电喷雾离子源(ESI)正离子方式扫描。结果显示,20种除草剂在对应质量浓度范围内线性良好,相关系数均不小于0.999 0,方法检出限为0.1~1.0 μg/kg,平均回收率为77.6%~115%,相对标准偏差为0.40%~3.8%。该方法简便快捷、灵敏度高、有机溶剂用量少,适用于实际样品中20种除草剂的高通量检测。
An optimized solvent-induced extraction pretreatment method combined with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was established for the simultaneous and rapid determination of 20 herbicides in agricultural soil. In the experiment,1.5 mL of dichloromethane was used as extractant,5 mL of acetonitrile as extractant,and 8 min vortex time were used for extraction,and ZORBAX Eclipse Plus C,18, column(100 mm×2.1 mm,1.8 μm) were used for separation,0.1% formic acid water and acetonitrile were used as mobile phase,and scanned with ESI mode. The results showed that 20 herbicides had good linearity in the corresponding mass concentration ranges with correlation coefficients not less than 0.999 0. The detection limit of the method ranged from 0.1-1.0 μg/kg,the average recoveries were 77.6%-115%,and the relative standard deviations were between 0.40%-3.8%. This method is simple,fast,sensitive,and requires less organic solvent,which is suitable for high-throughput detection of 20 herbicides in actual samples.
溶剂诱导萃取超高效液相色谱-串联质谱除草剂农田土壤
solvent-induced extractionUPLC-MS/MSherbicideagricultural soil
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