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首页> 外文期刊>International journal of environmental analytical chemistry >Residue screening in apple, grape and wine food samples for seven new pesticides using HPLC with UV detection. An application to trifloxystrobin dissipation in grape and wine
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Residue screening in apple, grape and wine food samples for seven new pesticides using HPLC with UV detection. An application to trifloxystrobin dissipation in grape and wine

机译:使用HPLC和UV检测在苹果,葡萄和葡萄酒食品样品中进行残留物筛查,以寻找7种新农药。葡萄和葡萄酒中三氟乙酸酯消散的应用

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摘要

A new analytical procedure was developed and validated, using liquid chromatography, for simultaneous determination of seven new pesticides belonging to different chemical classes (azoles, strobilurines, benzoylureas, and a new oxazolidinedione) in apple, grape and wine food samples. Solvent extraction of pesticides was performed using a cyclohexane-dichloromethane (9+1 v/v) mixture and the extract was cleaned-up by solid-phase extraction (SPE) using silica cartridges and elution with tetrahydrofurane. Separation of pesticides flusilazole, fenbuconazole, diniconazole, tebufenozide, famoxadone, trifloxystrobin and flufenoxuron was performed by gradient elution High-Performance Liquid Chromatography (HPLC) with a microbore Hypersil HS C_(18) column in 35 min total time, using mixtures of acetonitrile-water as the mobile phase. Pesticides were detected and quantified at 210 nm with a variable-wavelength UV detector. Recoveries of pesticides from spiked samples, at 0.05-2.0 mg kg~(-1) for apple and grape and at 0.025-0.250 mg L~(-1) for wine, ranged from 82 to 107% for apple and grape and from 87% to 106% for wine with RSD < 12%. The limits of quantification (LOQs) of the method, as a signal to noise ratio equalled 10, ranged from 0.02 to 0.10 mg kg~(-1) for apple and grape and from 0.005 to 0.02 mg L~(-1) for wine samples. The uncertainty associated with the analytical methodology, estimated using the 'bottom-up' approach, was lower than 12.8% for all pesticides and matrices tested. The proposed methodology was applied for the evaluation of trifloxystrobin residue levels in grapes exposed to field treatments and in the must and wine produced from them.
机译:开发了一种新的分析程序,并使用液相色谱法进行了验证,该方法可同时测定苹果,葡萄和葡萄酒食品样品中的7种不同化学类别的农药(唑类,strobilurines,苯甲酰脲和一种新的恶唑烷二酮)。使用环己烷-二氯甲烷(9 + 1 v / v)混合物对农药进行溶剂萃取,并使用硅胶柱通过固相萃取(SPE)纯化萃取液,并用四氢呋喃洗脱。通过梯度洗脱高效液相色谱(HPLC)并在35分钟内使用微孔Hypersil HS C_(18)色谱柱,使用乙腈混合物,分离农药氟硅唑,芬布康唑,迪尼康唑,替布芬唑,法莫沙酮,三氟氧嘧啶和氟苯氧隆以水为流动相。使用可变波长紫外检测器检测农药并在210 nm处定量。从加标样品中的农药回收率,苹果和葡萄为0.05-2.0 mg kg〜(-1),葡萄酒为0.025-0.250 mg L〜(-1),苹果和葡萄为82%至107%,87为RSD <12%的葡萄酒为%至106%。该方法的信噪比等于10时,定量限(LOQs)对于苹果和葡萄为0.02至0.10 mg kg〜(-1),对于葡萄酒为0.005至0.02 mg L〜(-1)样品。使用“自下而上”的方法估算的与分析方法有关的不确定性低于所有所测试农药和基质的12.8%。所提出的方法被用于评估暴露于田间处理的葡萄,葡萄汁和由其生产的葡萄酒中的三氟草醚残留水平。

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