Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.
Anal Chim Acta. 2012 Feb 3;713:70-8. doi: 10.1016/j.aca.2011.11.030. Epub 2011 Nov 22.
In the present work a new, simple, rapid and environmentally friendly dispersive liquid-liquid microextraction (DLLME) method has been developed for extraction/preconcentration of some triazole pesticides in aqueous samples and in grape juice. The extract was analyzed with gas chromatography-flame ionization detection (GC-FID) or gas chromatography-mass spectrometry (GC-MS). The DLLME method was performed in a narrow-bore tube containing aqueous sample. Acetonitrile and a mixture of n-hexanol and n-hexane (75:25, v/v) were used as disperser and extraction solvents, respectively. The effect of several factors that influence performance of the method, including the chemical nature and volume of the disperser and extraction solvents, number of extraction, pH and salt addition, were investigated and optimized. Figures of merit such as linearity (r(2)>0.995), enrichment factors (EFs) (263-380), limits of detection (0.3-5 μg L(-1)) and quantification (0.9-16.7 μg L(-1)), and relative standard deviations (3.2-5%) of the proposed method were satisfactory for determination of the model analytes. The method was successfully applied for determination of target pesticides in grape juice and good recoveries (74-99%) were achieved for spiked samples. As compared with the conventional DLLME, the proposed DLLME method showed higher EFs and less environmental hazards with no need for centrifuging.
本工作开发了一种新的、简单、快速且环境友好的分散液液微萃取(DLLME)方法,用于萃取/预浓缩水样和葡萄汁中的一些三唑类农药。采用气相色谱-火焰离子化检测(GC-FID)或气相色谱-质谱(GC-MS)对萃取物进行分析。DLLME 方法在含有水样的细管中进行。乙腈和正己醇-正己烷(75:25,v/v)混合物分别用作分散剂和萃取溶剂。考察并优化了影响方法性能的多个因素,包括分散剂和萃取溶剂的化学性质和体积、萃取次数、pH 值和加盐。所提出方法的评价指标,如线性(r²>0.995)、富集因子(EF)(263-380)、检测限(0.3-5 μg L⁻¹)和定量限(0.9-16.7 μg L⁻¹)以及相对标准偏差(3.2-5%),均适用于目标分析物的测定。该方法成功应用于葡萄汁中目标农药的测定,加标样品的回收率为 74-99%。与传统的 DLLME 相比,所提出的 DLLME 方法具有更高的 EF 和更少的环境危害,无需离心。