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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Evaluation of the rotating disk sorptive extraction technique with polymeric sorbent for multiresidue determination of pesticides in water by ultra-high-performance liquid chromatography-tandem mass spectrometry
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Evaluation of the rotating disk sorptive extraction technique with polymeric sorbent for multiresidue determination of pesticides in water by ultra-high-performance liquid chromatography-tandem mass spectrometry

机译:用超高效液相色谱 - 串联质谱法评价聚合物吸附剂旋转盘吸附萃取技术对水中杀虫剂中的多种杀虫剂的测定

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The use of pesticides has been associated with the increase of productivity of crops and control of vectors that cause diseases. However, excessive use of these compounds can cause human health and environmental problems, especially regarding to water resources. In this work, a method for multiresidue determination of 62 pesticides in surface water using the rotating disk sorptive extraction (RDSE) technique for sample preparation and ultra-high-performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/IVIS) for analysis was optimized and validated. The parameters time and rotational disk velocity for the extraction step, types and amounts of sorbents, sample pH, ionic strength, time and velocity of the rotating disk in the desorption step, as well different desorption solvents were evaluated. The best results were obtained using 50 mL of sample, acidified at pH 2.0, and 2.5 g of sodium chloride. The selected velocity of rotation in the extraction step was 1600 rpm for 80 min. Inside the disk cavity, a small amount (20 mg) of the polymeric sorbent Oasis (R) HLB was used. The desorption step was performed immerging the disk in 3 mL of methanol and rotating the disk at 1600 rpm for 60 min. Procedural calibration curves showed linearity between 0.05 or 0.1-2 mu g L-1, with r(2) > 0.99 for all compounds. The method presented practical limit of quantification of 0.05 or 0.1 pg L-1 and suitable accuracy and precision, with recoveries from 70.1 to 119.9% and RSD <= 20% for the levels 0.05, 0.1, 0.5 and 2 mu g L-1. The validated method was applied to surface water samples from different river and residues of atrazine, azoxystrobin, clomazone, difenoconazole, epoxiconazole, propoxur, simazine and tebuconazole were found in the range of 0.06-0.35 mu gL(-1). The results indicate that the proposed method is suitable for the determination of pesticide residues in surface water, allowing an easy and simultaneously preparation of several samples with low material consumption. (C) 2017 Elsevier B.V. All rights reserved.
机译:农药的使用与作物生产率的增加和导致疾病的载体的控制有关。然而,过量使用这些化合物会导致人类健康和环境问题,特别是对水资源有关。在这项工作中,使用旋转盘吸附萃取(RDSE)技术用于样品制备和超高效液相色谱法测定地表水中62种农药的方法,具有用于分析的串联质谱(UHPLC-MS / IVIS)优化和验证。对于解吸步骤中的吸附剂的提取步骤,样品pH,离子强度,时间和旋转盘的样品,样品pH,离子强度,时间和速度的参数时间和旋转盘速度,除了不同的解吸溶剂中,旋转盘的旋转盘的时间和速度。使用50ml样品获得最佳结果,在pH2.0下酸化和2.5g氯化钠。萃取步骤中的所选旋转速度为1600rpm,80分钟。在盘腔内,使用少量(20mg)的聚合物吸附剂OASIS(R)HLB。在3ml甲醇中浸泡盘并以1600rpm旋转60分钟,进行解吸步骤。程序校准曲线显示出0.05或0.1-2μg1-1之间的线性度,用于所有化合物的R(2)> 0.99。该方法呈现了0.05或0.1pg L-1的定量实际限制和适当的精度和精度,回收率从70.1-119.9%,0.05,0.1,0.5和2μgl-1的RSD <= 20%。验证的方法应用于来自亚唑嗪,亚沙昔林,甲唑酮,苯甲唑,环氧喹啉,丙唑,Simazine和Tebuconazole的不同河水和残留物的地表水样中被发现在0.06-0.35μg(-1)的范围内。结果表明,该方法适用于测定地表水中的农药残留物,允许易于制备几种具有低材料消耗的样品。 (c)2017年Elsevier B.V.保留所有权利。

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