中文摘要:为实现农药残留高灵敏分析,本研究提出了一种新版本的大体积样本窄孔管固相萃取方法,并与分散液-液微萃取技术联合进行农药残留萃取。本方法已经用于对不同蔬菜(马铃薯,番茄,洋葱,大蒜,芹菜,萝卜,甜菜,胡萝卜)中农药(甲霜灵、吡氟禾草灵、炔草酯、禾草灵、和溴螨酯)残留微量富集提取,并采用气相色谱-火焰电离法进行检测。最佳条件下,检测线性范围为0.08-10000μg/L,富集因子范围为1702-4147,回收率为31-75 %,检测限范围为0.02-0.25μg/L,定量限范围为0.08-0.83μg/L,10和50μg/L浓度分析物的相对标准差分别为4-7% (n = 6) 和2-4% (n = 7),三种不同浓度回收率均在80-101%范围.
外文摘要:In this study a new version of solid phase extraction performed in a
narrow-bore tube using large volume of sample followed by dispersive
liquid-liquid microextraction has been proposed to achieve a high
sensitive analytical method. It has been Used for the extraction and
preconcentration of trace concentrations of some pesticides (metalaxyl,
haloxyfop-r-methyl, clodinafop-propargyl, diclofop-methyl, and
bromopropylate) in different vegetables (potato, tomato, onion, garlic,
celery, radish, beet, and carrot) followed by gas chromatography-flame
ionization detection. In the proposed method mg-level of a sorbent (C-8)
is mixed with a dispersive solvent (iso-propanol) and then dispersed
into an aqueous solution placed into a narrow-bore tube. By this action,
the sorbent passes through the solution in a short time instead of
passing the solution from the cartridge in conventional solid phase
extraction in a long time. To achieve high enrichment factors, an
appropriate organic solvent (acetonitrile) is used to elute the
compounds of interest from the sorbent for the following dispersive
liquid-liquid microextraction procedure. Some important parameters which
affect the extraction efficiency were studied. Under the optimum
extraction conditions, the method showed wide linear ranges (0.08-10,000
mu g L-1). Enrichment factors and extraction recoveries were in the
ranges of 1702-4147 and 31-75%, respectively. Detection limits were in
the range of 0.02-0.25 mu g L-1 in solution (0.01-0.89 mu g kg(-1) in
samples). LOQs were obtained in the range of 0.08-0.83 mu g L-1 in
solution (0.04-2.9 mu g kg(-1) in samples). Relative standard deviations
of 4-7% (n = 6) and 2-4% (n = 7) were obtained for 10 and 50 mu g L-1 of
each analyte, respectively. The relative recoveries obtained in three
different concentrations were 80-101%. (C) 2016 Elsevier B.V. All rights
reserved.
外文关键词:Dispersive liquid-liquid microextraction, Dispersive solid phase extraction, Gas chromatography, Sample preparation, Pesticides
作者:Farajzadeh, Mir Ali; Yadeghari, Adeleh; Khoshmaram, Leila
作者单位:Univ Tabriz, Dept Analyt Chem, Fac Chem, Tabriz, Iran.
期刊名称:MICROCHEMICAL JOURNAL
期刊影响因子:2.893
出版年份:2017
出版刊次:3
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