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涡旋辅助表面活性剂强化乳化液液微萃取。

Vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction.

机构信息

Department of Applied Chemistry, China Agricultural University, Beijing 100193, China.

出版信息

J Chromatogr A. 2011 Oct 7;1218(40):7071-7. doi: 10.1016/j.chroma.2011.08.029. Epub 2011 Aug 17.

Abstract

A novel sample pre-treatment technique, based on vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction (VSLLME), followed by gas chromatography-flame photometric detection (GC-FPD) has been developed for the determination of seven organophosphorus pesticides (OPPs) in wine and honey samples. In the VSLLME method, the extraction solvent was dispersed into the aqueous samples by the assistance of vortex agitator. Meanwhile, the addition of a surfactant, which was used as an emulsifier, could enhance the speed of the mass-transfer from aqueous samples to the extraction solvent. The main parameters relevant to this method were investigated and the optimum conditions were established: 15 μL chlorobenzene was used as extraction solvent, 0.2 mmol L(-1) Triton X-114 was selected as the surfactant, the extraction time was fixed at 30s, 3% sodium chloride was added and the extraction process was performed under the room temperature. Under the optimum conditions, limits of detections (LODs) were varied between 0.01 and 0.05 μg L(-1). The relative standard deviation (RSD, n=6) ranged from 2.3% and 8.9%. The linearity was obtained by five points in the concentration range of 0.1-50.0 μg L(-1). Correlation coefficients (r) varied from 0.9969 to 0.9991. The enrichment factors (EFs) were in a range of 282-309. Finally, the proposed method has been successfully applied to the determination of target analytes in real samples. The recoveries of the target analytes in wine and honey samples were between 81.2% and 108.0%.

摘要

一种基于涡旋辅助表面活性剂增强乳化液液微萃取(VSLLME)的新型样品预处理技术,结合气相色谱-火焰光度检测(GC-FPD),已被开发用于测定葡萄酒和蜂蜜样品中的七种有机磷农药(OPPs)。在 VSLLME 方法中,萃取溶剂在涡旋搅拌器的辅助下分散到水样中。同时,添加表面活性剂(用作乳化剂)可以加快从水样到萃取溶剂的质量转移速度。对该方法的主要参数进行了考察,并确定了最佳条件:使用 15μL 氯苯作为萃取溶剂,选择 0.2mmol L(-1) Triton X-114 作为表面活性剂,萃取时间固定为 30s,加入 3%氯化钠,萃取过程在室温下进行。在最佳条件下,检测限(LOD)在 0.01 至 0.05μg L(-1)之间变化。相对标准偏差(RSD,n=6)范围为 2.3%至 8.9%。在 0.1-50.0μg L(-1)的浓度范围内,通过五点得到了线性关系。相关系数(r)在 0.9969 至 0.9991 之间变化。富集因子(EF)在 282-309 之间。最后,该方法成功应用于实际样品中目标分析物的测定。在葡萄酒和蜂蜜样品中,目标分析物的回收率在 81.2%至 108.0%之间。

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