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Microwave-assisted steam distillation for the determination of organochlorine pesticides and pyrethroids in Chinese teas

机译:微波辅助水蒸气蒸馏法测定中国茶中有机氯农药和拟除虫菊酯

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In this work, microwave-assisted steam distillation (MASD) extraction method followed by gas chromatography/electron capture detection (GC/ECD) was developed for the determination of organochlorine pesticides (OCPs) and pyrethroids in the Chinese teas. MASD is a combination of microwave-assisted extraction (MAE) and steam distillation techniques. Water vapor generated by microwave irradiation is used to accelerate desorption of the analytes from the sample, and the nonpolar organic solvent used for trapping the analytes is kept from direct contact with the sample by the water. Therefore, relatively clean extracts were obtained compared to the method directly using organic solvent as extraction solvent, such as ultrasonic extraction (USE). Microwave power of 200 W and irradiation time of 2 min was found to be the optimum conditions for the MASD process, and n-heptane was chosen as the analyte-trapping solvent in the study. Five OCPs (alpha-HCH, gamma-HCH, dicofol, p,p'-DDE, p,p'-DDT) and two pyrethroids (bifenthrin, fenvalate) were determined using this extraction method in the tea samples. The relative standard deviation (R.S.D.) of the analytes varied from 2.2 to 8.4%, and the method detection limits (MDLs) found were lower than 0.23 mu g/kg. The recoveries of the seven compounds in the Jasmine tea sample were between 84.04 and 110.1%. Comparative results obtained by MASD and USE were also discussed in the study. (c) 2006 Elsevier B.V. All rights reserved.
机译:在这项工作中,开发了微波辅助蒸汽蒸馏(MASD)提取方法,然后进行气相色谱/电子捕获检测(GC / ECD)方法,用于测定中国茶中的有机氯农药(OCP)和拟除虫菊酯。 MASD是微波辅助萃取(MAE)和蒸汽蒸馏技术的结合。通过微波辐射产生的水蒸气被用来加速分析物从样品中的解吸,并且用于捕获分析物的非极性有机溶剂被阻止与水直接接触。因此,与直接使用有机溶剂作为萃取溶剂的方法(例如超声萃取(USE))相比,可获得相对清洁的萃取物。发现200 W的微波功率和2分钟的照射时间是MASD工艺的最佳条件,并且在研究中选择了正庚烷作为捕获分析物的溶剂。使用这种提取方法,在茶叶样品中确定了五个OCP(α-HCH,γ-HCH,三氯杀螨醇,三氯杀螨醇,p,p'-DDE,p,p'-DDT)和两个拟除虫菊酯(联苯菊酯,fenvalate)。分析物的相对标准偏差(R.S.D.)在2.2%至8.4%之间变化,发现的方法检测限(MDL)低于0.23μg / kg。茉莉花茶样品中的7种化合物的回收率在84.04和110.1%之间。在研究中还讨论了通过MASD和USE获得的比较结果。 (c)2006 Elsevier B.V.保留所有权利。

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