Sanchez-Ortega A, Unceta N, Gómez-Caballero A, Sampedro M C, Akesolo U, Goicolea M A, Barrio R J
Departament of Analytical Chemistry. Faculty of Pharmacy, University of the Basque Country, 01006 Vitoria-Gasteiz, Spain.
Anal Chim Acta. 2009 May 8;641(1-2):110-6. doi: 10.1016/j.aca.2009.03.044. Epub 2009 Apr 5.
An automated thermal desorption-gas chromatography-mass spectrometry method for the determination of triazin herbicides in aqueous solution with excellent sensitivity was developed. The method is based on the use of stir bar sorptive extraction. The main parameters such as extraction time, sample volume, the addition of salt and organic modifiers, desorption temperature, desorption flow and desorption time which affect the efficiency of the proposed methodology are fully discussed. The proposed method is sensitive and shows a good linearity within a range of 10-10000 ng L(-1) with correlation coefficients higher than 0.998. Quantitation limits are, in all cases, below the limits accepted by European legislation for human waters consumption and ranging between 11.3 ng L(-1) and 0.7 ng L(-1). The repetitivity, expressed as a relative standard deviation, has values of lower than 8% for all analytes. Using this method, determination of 10 triazines in underground water samples was successfully performed. The average concentrations obtained in the analysis of the spiked samples at two different levels of concentration correspond to mean recoveries ranging from 94.4+/-5.1% to 106.0+/-6.3% for a significance level of 0.05.
建立了一种用于测定水溶液中三嗪类除草剂的自动热解吸-气相色谱-质谱法,该方法具有出色的灵敏度。该方法基于搅拌棒吸附萃取技术。充分讨论了影响所提出方法效率的主要参数,如萃取时间、样品体积、盐和有机改性剂的添加量、解吸温度、解吸流速和解吸时间。所提出的方法灵敏,在10 - 10000 ng L⁻¹范围内具有良好的线性,相关系数高于0.998。在所有情况下,定量限均低于欧洲人类用水立法所接受的限值,范围在11.3 ng L⁻¹至0.7 ng L⁻¹之间。以相对标准偏差表示的重复性,所有分析物的值均低于8%。使用该方法成功地对地下水样品中的10种三嗪进行了测定。在两种不同浓度水平的加标样品分析中获得的平均浓度,对于0.05的显著性水平,平均回收率在94.4±5.1%至106.0±6.3%之间。