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Dispersive solid phase extraction combined with solidification of floating organic drop-liquid-liquid microextraction using in situ formation of deep eutectic solvent for extraction of phytosterols from edible oil samples.
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2020-09-01 , DOI: 10.1016/j.chroma.2020.461523
Mohammad Reza Afshar Mogaddam 1 , Mir Ali Farajzadeh 2 , Sodeif Azadmard Damirchi 3 , Mahboob Nemati 4
Affiliation  

In this study, a dispersive solid phase extraction method was combined with solidification of floating organic drop–liquid–liquid microextraction based on in situ synthesis of deep eutectic solvent. It was used for the extraction of some phytosterols from edible oil samples. The extracted analytes were quantified by gas chromatography–mass spectrometry. In this procedure, the sample lipids are saponified with sodium hydroxide and then the analytes are adsorbed onto an octadecylsilane sorbent. After that the analytes are desorbed from the sorbent with ethanol as an elution solvent and the eluant is diluted with deionized water to obtain a homogenous solution. Then, a few amounts of choline chloride and n-butyric acid are dissolved in the solution and transferred into a water batch adjusted at 75 ⁰C for 5 min. During this period Choline chloride and n-butyric acid form a deep eutectic solvent (extraction solvent) dispersed in whole parts of the solution. The obtained cloudy solution is placed into an ice bath. The extraction solvent is collected and solidified on the top of the solution. Finally, it is removed and allows melted at room temperature and an aliquat 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 0.52–1.6 and 1.7–5.6 ng mL–1, respectively. Enrichment factors and extraction recoveries of the analytes ranged from 312 to 375 and 75–90%, respectively. The method had a proper percision with relative standard deviations less than ≤8.2% for intra– (n = 6) and inter–day (n = 6) precisions at a concentration of 15 ng mL–1 of each analyte. Finally the method was successfully used for determination of the analytes in some edible oil samples.



中文翻译:

分散固相萃取结合浮法有机液滴-液体-液体微萃取的固化,使用原位形成的深共晶溶剂从食用油样品中提取植物甾醇。

在这项研究中,基于深共晶溶剂的原位合成,将分散固相萃取方法与浮动有机液滴-液-液微萃取的固化相结合。它用于从食用油样品中提取一些植物甾醇。提取的分析物通过气相色谱-质谱法定量。在该程序中,将样品脂质用氢氧化钠皂化,然后将分析物吸附到十八烷基硅烷吸附剂上。之后,将分析物用乙醇作为洗脱溶剂从吸附剂中解吸,并将洗脱液用去离子水稀释,得到均质溶液。然后,一些量的氯化胆碱和Ñ将丁酸溶解在溶液中,并转移到75℃下调节5分钟的水批次中。在此期间,氯化胆碱和丁酸形成一种深的低共熔溶剂(萃取溶剂),分散在整个溶液中。将获得的浑浊溶液置于冰浴中。收集萃取溶剂,并在溶液顶部固化。最后,将其除去并使其在室温下熔化,然后将等量溶液注入分离系统中。该方法的验证表明,检测和定量限在0.52–1.6和1.7–5.6 ng mL –1范围内, 分别。分析物的富集因子和提取回收率分别为312%至375%和75-90%。该方法具有适当的 精密度,当每种分析物的浓度为15 ng mL –1时,内(n  = 6)和日间(n = 6)精度的相对标准偏差均小于或等于8.2%。最终,该方法成功地用于测定某些食用油样品中的分析物。

更新日期:2020-09-11
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