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采用固相微萃取-气相色谱-电子捕获检测法测定地下水样中的有机氯农药

Determination of organochlorine pesticides in ground water samples using solid-phase microextraction by gas chromatography-electron capture detection.

作者信息

Raposo Júnior Jorge Luiz, Ré-Poppi Nilva

机构信息

Departamento de Química, Centro de Ciências Exatas e Tecnologia, UFMS, CP 549, 79070-900 Campo Grande, MS, Brazil.

出版信息

Talanta. 2007 Jul 31;72(5):1833-41. doi: 10.1016/j.talanta.2007.02.024. Epub 2007 Feb 22.

Abstract

A direct immersion solid-phase microextraction coupled with gas chromatography-electron capture detection (SPME-GC-ECD) method was optimized and validated for the quantitative determination of 18 organochlorine pesticides in ground water. Ionic strength, stirring speed, adsorption and desorption time and pH were some of the parameters investigated in order to select the optimum conditions for SPME with a 50/30 DVB/CAR/PDMS fiber coating. The SPME-GC/ECD method showed good linear response below 10 ng L(-1) with R(2) values in the range of 0.9950-0.9997. The repeatability of the measurements were lower than 10%. Values of relative recoveries located within the acceptable range (80-120%). Limits of quantification (LOQ) from 4.5x10(-3) to 1.5 ng L(-1) were obtained. On average 8 organochlorines were found per sample, even so all the 18 organochlorines were quantified among them. Substances such as endrin ketone, gamma-BHC and beta-BHC were the pesticides determined in larger concentration (0.06-305 ng L(-1)), while methoxychlor and aldrin in smaller amounts (0.151-1.55 ng L(-1)). Measured levels of organochlorine pesticides were above the limits established by Brazilian regulations.

摘要

优化并验证了一种直接浸入式固相微萃取结合气相色谱 - 电子捕获检测(SPME - GC - ECD)方法,用于定量测定地下水中的18种有机氯农药。研究了离子强度、搅拌速度、吸附和解吸时间以及pH值等参数,以便为使用50/30 DVB/CAR/PDMS纤维涂层的SPME选择最佳条件。SPME - GC/ECD方法在10 ng L⁻¹以下显示出良好的线性响应,R²值在0.9950 - 0.9997范围内。测量的重复性低于10%。相对回收率值在可接受范围内(80 - 120%)。获得的定量限(LOQ)为4.5×10⁻³至1.5 ng L⁻¹。每个样品平均发现8种有机氯,即便如此,所有18种有机氯都在其中被定量。异狄氏剂酮、γ - 六六六和β - 六六六等物质是浓度较高(0.06 - 305 ng L⁻¹)的农药,而甲氧滴滴涕和艾氏剂含量较少(0.151 - 1.55 ng L⁻¹)。所测有机氯农药水平高于巴西法规规定的限值。

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