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程功 沈阳农业大学 植物保护学院, 沈阳 110866  
刘娜 沈阳农业大学 植物保护学院, 沈阳 110866  
田宏哲 沈阳农业大学 植物保护学院, 沈阳 110866  
朱赫 沈阳农业大学 植物保护学院, 沈阳 110866  
纪明山 沈阳农业大学 植物保护学院, 沈阳 110866 jimingshan@163.com 
中文摘要:建立了QuEChERS-高效液相色谱-串联质谱(QuEChERS-HPLC-MS/MS)测定丙炔氟草胺在食品(苹果、葡萄、柑橘、甘蓝、小麦、大豆)、土壤和水中残留量的方法,并分析了其在土壤中的消解动态。样品经乙腈均质提取,采用C18N-丙基乙二胺(PSA)、石墨化碳黑(GCB)和无水硫酸镁混合净化剂分散萃取处理,以C18色谱柱分离,采用电喷雾正离子(ESI+)扫描,多反应监测模式(MRM)检测,基质匹配标准溶液外标法定量。结果表明:在0.01~5 mg/kg范围内,丙炔氟草胺在苹果、葡萄、柑橘、甘蓝、小麦、大豆、土壤及水8种基质中的峰面积与其质量浓度间呈良好的线性关系(R2 > 0.997 6)。在0.01、0.1和1 mg/kg添加水平下,丙炔氟草胺在8种基质中的日内平均回收率为82%~104%,相对标准偏差(RSD)(n = 5)为1.1%~7.8%;日间平均回收率为77%~109%,RSD(n = 15)为0.1%~9.2%。方法的定量限(LOQ)为0.000 3~0.003 2 mg/kg,均低于美国、中国、日本及欧盟等国家和地区的最大残留限量值(MRLs)。本方法简便、稳定、灵敏,能够满足实际检测需求。同时,对大田土壤分析的结果表明,丙炔氟草胺在土壤中的半衰期为23.9 d,属易降解农药。
中文关键词:QuEChERS  高效液相色谱-串联质谱  丙炔氟草胺  食品  土壤    残留  消解
Residue analysis of flumioxazin in food and environment by modified QuEChERS method using high performance liquid chromatography-tandem mass spectrometry and the dissipation dynamics in soil
Abstract:A rapid, simple, sensitive and effective analytical method for the determination of flumioxazin in food (apple, grape, wheat, soybean, cabbage, and orange), soil and water based on a QuEChERS procedure was developed using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The samples were extracted with acetonitrile and cleaned-up by dSPE with C18, GCB, PSA mixed with MgSO4 as sorbent in different matrices. The samples were detected by using an Eclipse Plus C18 column connected to an electrospray ionization source in positive mode (ESI+), monitoring(MRM) mode. The matrix-matched external standard calibration curves were used for quantitative analysis. The results showed that the linearity of flumioxazin in the range of 0.01-5 mg/kg, with determination coefficients higher than 0.997 6. The intra-day average recoveries ranged from 82%-104% in eight matrices at three levels (0.01, 0.1 and 1 mg/kg) and the relative standard deviation (RSD) ranged from 1.1%-7.8% (n = 5). The inter-day average recoveries ranged from 77%-109% in eight matrices at three levels (0.01, 0.1 and 1 mg/kg) and the RSD ranged from 0.1%-9.2% (n = 15). The LOQs ranged from 0.000 3-0.003 2 mg/kg, which were lower than the maximum residue limits (MRLs) of flumioxazin established by America, the European Union, Japan, and China. It can detect the residues of flumioxazin in food and environmental samples. Based on this method, the dissipation dynamics of flumioxazin in the field soil was characterized, which provided a theoretical basis for the risk assessment of food safety and environment pollution.
Key words:QuEChERS  high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)  flumioxazin  food  soil  water  residue  dissipation
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