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首页> 外文期刊>Journal of the Brazilian Chemical Society >Development of MSPD method for the determination of pesticide residues in tomato by GC-MS
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Development of MSPD method for the determination of pesticide residues in tomato by GC-MS

机译:气相色谱-质谱法测定番茄中农药残留的MSPD方法的建立

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A simple and effective extraction method based on matrix solid-phase dispersion was developed to determine dimethoate, methyl-parathion, malathion, tebuconazole and cypermethrin in tomato using gas chromatography-mass spectrometry and selected ion monitoring (GC-MS, SIM). Different parameters of the method were evaluated, such as type of solid phase (C18, alumina, sílica-gel and Florisil), the amount of solid phase and eluent [dichloromethane, ethyl acetate, n-hexane and n-hexane:ethyl acetate (1:1 and 1:3, v/v)]. The best results were obtained using 2.0 g of tomato, 0.5 g of alumina as dispersant sorbent, 0.5 g of Florisil as clean-up sorbent and dichloromethane as eluting solvent. The method was validated by fortified tomato samples at different concentration levels (0.05 to 4.0 mg kg-1). Average recoveries (7 replicates) ranged from 77% to 100% with relative standard deviation between 3.7% and 12.9%. Detection and quantification limits ranged from 0.01 to 0.02 mg kg-1 and 0.03 to 0.06 mg kg-1 for the whole fruit of tomato, respectively. The proposed method was applied to analyze of these compounds in commercial tomato samples and residues of methyl-parathion, dimethoate and malathion were detected on the tomato samples at concentrations below the maximum residue levels (MRLs) established by Brazilian legislation and Codex Alimentarius.
机译:建立了一种基于基质固相分散的简单有效的提取方法,采用气相色谱-质谱和选定的离子监测(GC-MS,SIM)方法测定番茄中的乐果,甲基对硫磷,马拉硫磷,戊唑醇和氯氰菊酯。评估了该方法的不同参数,例如固相类型(C18,氧化铝,硅凝胶和Florisil),固相和洗脱液的量[二氯甲烷,乙酸乙酯,正己烷和正己烷:乙酸乙酯( 1:1和1:3,v / v)]。使用2.0 g番茄,0.5 g氧化铝作为分散剂吸附剂,0.5 g Florisil作为净化吸附剂和二氯甲烷作为洗脱溶剂,可获得最佳结果。通过不同浓度水平(0.05至4.0 mg kg-1)的强化番茄样品验证了该方法的有效性。平均回收率(7次重复)的范围从77%到100%,相对标准偏差在3.7%和12.9%之间。整个番茄果实的检出限和定量限分别为0.01至0.02 mg kg-1和0.03至0.06 mg kg-1。拟议的方法用于分析商业番茄样品中的这些化合物,并以低于巴西法律和食品法典规定的最大残留水平(MRL)的浓度检测到番茄样品中的对硫磷,乐果和马拉硫磷的残留。

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