快速溶剂提取-GC-MS/MS法测定土壤中三唑磷、螺螨酯、异菌脲、氰氟草酯和多效唑
朱文霞
山东省临沂生态环境监测中心，山东临沂 276000
Determination of triazophos, spiroides, isocarbazide, cyhalofovir and paclobutrazol in soil by rapid solvent extraction-GC-MS/MS
ZHU Wenxia
Shandong Linyi Ecological Environment Monitoring Center, Linyi 276000, China
摘要：建立快速溶剂萃取-气相色谱-串联质谱法测定土壤中三唑磷、螺螨酯、异菌脲、氰氟草酯和多效唑微量残留的分析方法。随机采集土壤样品，自然风干，粉碎，过筛，置于快速溶剂萃取池中，用丙酮提取，提取液置于氮吹仪中吹至近干，用丙酮复溶，过0.45 μm滤膜后进样测定，外标法定量。5种农药的质量浓度在0.02～4.0 μg/mL范围内与色谱峰面积具有良好的线性关系，相关系数均大于0.997，检出限为0.002～0.005 mg/kg。样品在0.2，1.0，3.0 mg/kg 3个加标水平时的回收率为89.8%～102.5%，测定结果的相对标准偏差为2.78％～4.03％(n=6)。该方法自动化程度高，定性定量结果准确，重复性好，适用于土壤中多种农药残留的测定。
Abstract：A method for the determination of triazophos, spirodiclofen, isocarburon, cyhalofop and paclobutrazol residues in soil by rapid solvent extraction-gas chromatography-tandem mass spectrometry was established. The soil samples were collected randomly, dried naturally, crushed, sieved, then transferred to rapid solvent extraction pond, and extracted with acetone. The extraction solution was put into the nitrogen blower until it was nearly dry, and then redissolved with acetone. After passing the 0.45 μm filter membrane, the sample was injected for determination, and the external standard method was used for quantitative determination. The mass concentration of five pesticides had a good linear relationships with the chromatographic peak area in the range of 0.02-4.0 µg/mL, the correlation coefficients were all more than 0.997, and the detection limits were 0.002-0.005 mg/kg. The recoveries of standard addition in three different levels (0.2, 1.0, 3.0 mg/kg) were 89.8%-102.5%, and the relative standard deviations were 2.78%-4.03%(n=6). The method is high degree of automation, accurate qualitative and quantitative results and good repeatability, it is suitable for the determination of pesticide residues in soil.
关键词：加速溶剂萃取；气相色谱-串联质谱法；土壤；农药残留
Keywords：rapid solvent extraction; gas chromatography-tandem mass spectrometry; soil; pesticide residue
本文引用格式：
朱文霞.快速溶剂提取-GC-MS/MS法测定土壤中三唑磷、螺螨酯、异菌脲、氰氟草酯和多效唑[J].化学分析计量，2020，29(6)：71-74.
ZHU W X. Determination of triazophos，spiroides，isocarbazide，cyhalofovir and paclobutrazol in soil by rapid solvent extraction-GC-MS/MS[J]. Chemical analysis and meterage，2020，29(6)：71-74.
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