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Determination of tridemorph and other fungicide residues in fruit samples by liquid chromatography-electrospray tandem mass spectrometry

机译:液相色谱-电喷雾串联质谱法测定水果样品中的三聚体和其他杀菌剂残留

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A rapid and sensitive liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS-MS) method for the determination of tridemorph and other pre- and post-harvest fungicides (carbendazim, thiabendazole, imazalil, propiconazole and bitertanol) in banana and orange samples has been developed and validated. The sample preparation was a simple extraction step with acetone using a high-speed blender prior to the injection of the five-fold diluted extract into the LC system with no other previous sample pre-treatment. Quantification was carried out using a matrix matched calibration curve which was linear in the range of 1-100 ng ml(-1) for all the compounds. The limit of quantification was 0.05 mg kg(-1) for all studied compounds, whereas limits of detection ranged between 0.005 and 0.025 mg kg(-1) (0.01 mg kg(-1) for tridemorph). Recoveries for tridemorph from spiked banana and orange samples at 0.05 and 1 mg kg(-1) were satisfactory, with values between 83 and 99% and relative standard deviations (R.S.D.s) lower than 13% (n = 5). For the other fungicides, recoveries between 75 and 95% with R.S.D.s lower than 12% were obtained. The developed method has been applied to the determination of selected fungicides in real samples of bananas and oranges from different origin. Thiabendazole and imazalil have been detected in almost all orange samples analyzed, and in around of 30% of banana samples. Bitertanol residues exceeded the maximum residue level (0.05 mg kg(-1)) in three banana samples while tridemorph was only detected in one sample. (C) 2004 Elsevier B.V. All rights reserved.
机译:快速灵敏的液相色谱-电喷雾电离串联质谱(LC-ESI-MS-MS)方法测定香蕉中的三苯甲基及其他收获前和收获后的杀菌剂(多菌灵,噻菌灵,咪唑,丙环唑和比替洛尔)橙色样品已经开发和验证。样品制备是使用高速混合器用丙酮进行的简单萃取步骤,然后将五倍稀释的萃取液注入LC系统,而无需进行其他先前的样品预处理。使用基质匹配的校准曲线进行定量,对于所有化合物,校准曲线在1-100 ng ml(-1)范围内呈线性关系。所有研究的化合物的定量限为0.05 mg kg(-1),而检出限为0.005至0.025 mg kg(-1)(对于tridemorph为0.01 mg kg(-1))。从加标的香蕉和橙子样品中0.05和1 mg kg(-1)的三叉晶的回收率令人满意,其值在83%至99%之间,相对标准偏差(R.S.D.s)低于13%(n = 5)。对于其他杀菌剂,回收率在75%至95%之间,R.S.D。低于12%。所开发的方法已用于测定不同来源的香蕉和橙子的真实样品中的选定杀真菌剂。在几乎所有分析的橙色样品中以及大约30%的香蕉样品中都检测到了噻菌灵和咪唑唑。在三个香蕉样品中,Bitertanol残留量超过最大残留量(0.05 mg kg(-1)),而仅在一个样品中检测到tridemorph。 (C)2004 Elsevier B.V.保留所有权利。

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