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Combination of dispersive solid phase extraction with solidification organic drop-dispersive liquid-liquid microextraction based on deep eutectic solvent for extraction of organophosphorous pesticides from edible oil samples.
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2020-07-06 , DOI: 10.1016/j.chroma.2020.461390
Elham Zahiri 1 , Jalil Khandaghi 1 , Mir Ali Farajzadeh 2 , Mohammad Reza Afshar Mogaddam 3
Affiliation  

A dispersive solid phase extraction method was combined with deep eutectic solvent–based solidification of floating organic drop–dispersive liquid–liquid microextraction and used for the extraction/preconcentration of some organophosphorus pesticides residues from edible oil samples. The extracted analytes were quantified with gas chromatography–nitrogen phosphorous detector. In this procedure, the sample lipids are saponified with a sodium hydroxide solution and then the analytes are adsorbed onto a primary secondary amine sorbent. After that the analytes are desorbed with acetone as an elution/dispersive solvent and mixed with choline chloride: 3,3–dimethyl butyric acid deep eutectic solvent and the mixture is rapidly dispersed into deionized water. Then, the obtained cloudy solution is centrifuged and placed into an ice bath. The extraction solvent is solidified on the top of the solution. Finally, it is removed and dissolved in acetonitrile, and 1 µL of the solution is injected into the separation system. Validation of the method showed that limits of detection and quantification were in the ranges of 0.06–0.24 and 0.20–0.56 ng mL–1, respectively. Enrichment factors and extraction recoveries of the analytes ranged from 170–192 and 68–77%, respectively. The method had an acceptable precision with relative standard deviations less than ≤9.2% for intra– (n=6) and inter–day (n=6) precisions at four concentrations (3, 10, 50, and 250 ng mL–1, each analyte). Finally the method was used for determination of the analytes in five edible oil samples.



中文翻译:

基于深共熔溶剂的分散固相萃取与固化有机滴-分散液-液微萃取相结合,从食用油样品中萃取有机磷农药。

分散固相萃取方法与基于深共熔溶剂的漂浮有机液滴-分散液-液微萃取的凝固相结合,用于从食用油样品中萃取/浓缩一些有机磷农药残留物。提取的分析物通过气相色谱-氮磷检测器进行定量。在该程序中,将样品脂质用氢氧化钠溶液皂化,然后将分析物吸附到伯仲胺吸附剂上。之后,将分析物用丙酮作为洗脱剂/分散剂解吸,并与氯化胆碱:3,3-二甲基丁酸深共熔溶剂混合,然后将混合物迅速分散到去离子水中。然后,将获得的浑浊溶液离心并置于冰浴中。萃取溶剂在溶液顶部固化。最后,将其除去并溶于乙腈,然后将1 µL溶液注入分离系统。方法的验证表明检测限和定量限在0.06-0.24和0.20-0.56 ng mL范围内分别为–1。分析物的富集因子和提取回收率分别为170-192和68-77%。该方法具有可接受的精确度,相对标准偏差为帧内小于≤9.2%(N = 6)和日间(N = 6)精度在四个浓度(3,10,50,和250纳克毫升-1,每种分析物)。最后,该方法用于测定五个食用油样品中的分析物。

更新日期:2020-07-13
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