Method for Residues Analysis of Isoxaflutole and Its Metabolites in Maize

Mao Jia, Feng Yizhi, Qi Xiaoxue, Han Jifeng, Pan Jinju, Liang Lin, Liu Wei, Zuo Bojun
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Abstract

A rapid and sensitive analytical method for the determination of isoxaflutole and diketonitrile (DKN) residues in maize was established based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and high performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS). The samples were extracted with acetonitrile and purified with octadecylsilane (C18). The mass spectrometer was performed in multi-reaction monitoring mode, and electrospray ionization in negative mode was selected. The isoxaflutole and DKN residues were quantified by the external standard method using the matched standard solution to compensate for matrix effect. The results indicated that the calibration curves of isoxaflutole and DKN were linear in the range of 0.005-0.5mg/L with correlation coefficients of more than 0.9922. When the addition level ranged from 0.01 to 0.1mg/kg the average recoveries of isoxaflutole and DKN in maize, green maize and straw were 95%-108%, and the relative standard deviation (RSD) ranged from 2% to 11%. The limit of quantitation (LOQ) were 0.01 mg/kg in different matrices. This method has many characteristics, such as simple, rapid and accurate, and can be adapted for the confirmation of isoxaflutole and DKN residues in maize samples.
玉米中异草氟唑及其代谢物残留分析方法
建立了一种基于QuEChERS(快速、简便、廉价、有效、坚固、安全)和高效液相色谱-串联质谱(HPLC-MS/MS)的玉米中异草氟唑和二酮腈(DKN)残留快速、灵敏的分析方法。样品用乙腈提取,用十八烷基硅烷(C18)纯化。质谱计采用多反应监测模式,电喷雾电离选择负极模式。采用外标法对异氟吕酮和DKN的残留量进行定量,采用匹配的标准溶液补偿基质效应。结果表明:异草柳酮与DKN在0.005 ~ 0.5mg/L范围内线性良好,相关系数均大于0.9922;当添加量为0.01 ~ 0.1mg/kg时,玉米、绿玉米和秸秆中异草氟唑和DKN的平均加样回收率为95% ~ 108%,相对标准偏差(RSD)为2% ~ 11%。不同基质的定量限均为0.01 mg/kg。该方法具有简便、快速、准确等特点,适用于玉米样品中异草氟唑和DKN残留的确证。
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