Determination of five aphid control drugs in soil by gas chromatography-tandem mass spectrometry
Lianyungang Guannan Ecological Environment Monitoring Station, Lianyungang 222500, China
摘要：建立测定土壤中抗蚜威、噻虫嗪、啶虫脒、联苯菊酯和噻嗪酮5种农药残留的气相色谱-串联质谱法。称取10.0 g预处理后的土壤样品，置于50 mL离心管中，依次加入8.0 mL纯化水、25 mL乙腈、2.0 g氯化钠，旋涡混合并强力振摇1 min，冷冻离心5 min。取上清液，置于25 mL净化管中，涡旋混匀1 min，冷冻离心5 min。准确移取10.0 mL上清液，浓缩至近干，加入1.0 mL正己烷溶解，溶液经0.22μm滤膜过滤后，采用气相色谱-串联质谱法测定，校正曲线外标法定量。抗蚜威、噻虫嗪、啶虫脒、联苯菊酯和噻嗪酮的质量浓度在0.02～2.0?g/mL范围内与色谱峰面积线性关系良好，相关系数均大于0.995，检出限分别为0.005 0、0.005 8、0.004 2、0.008 0和0.004 7 mg/kg。3种加标质量浓度水平的回收率为85.7%～103.7%，测定结果的相对标准偏差均小于5.0%(n=6)。该方法样品处理简单，溶剂用量少，净化效果好，定性、定量结果准确。
Abstract：A gas chromatography-tandem mass spectrometry was established for the determination of five pesticide residues including pirimicarb, thiamethoxam, acetamiprid, bifenthrin and thiazinone in soil. 10.0 g pretreated soil sample was added into a 50 mL centrifuge tube, then 8.0 mL of purified water, 25 mL of acetonitrile and 2.0 g of sodium chloride were added in sequence, vortex mixed and shook strongly for 1 min, and froze centrifuge for 5 min. The supernatant was put into a 25 mL puri fication tube, vortex mixed for 1 min, froze and centrifuge for 5 min. 10.0 mL of supernatant was concentrated to nearly dry, and added 1.0 mL of -hexane to dissolve. After the solution was filtered with 0.22μm filter membrane, determined by gas chromatography tandem mass spectrometry and quantified by calibration curve external standard method. The mass concentrations of pirimicarb, thiamethoxam, acetamiprid, bifenthrin and buprofezin had a good linear relationship in the range of 0.02-2.0μg/mL with the correlation coefficients all greater than 0.995, and the detection limits were 0.005 0, 0.005 8, 0.004 2, 0.008 0 and 0.004 7 mg/kg, respectively. The recoveries of three spiked mass concentration levels were 85.7%-103.7%, the relative standard deviations of the determination results were all less than n 5.0%(n=6). This method has the advantages of simple operation, less solvent usage, good purification effect and accurate qualitative and quantitative results.
Keywords：gas chromatography-tandem mass spectrometry; soil; pesticide; pirimicarb; thiamethoxam; acetamiprid;bifenthrin; thiazinone
PAN Zhengyi. Determination of five aphid control drugs in soil by gas chromatography-tandem mass spectrometry[J]. Chemical Analysis and Meterage，2022，31(7)：58.