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采用分散液液微萃取-浮动有机液滴固化法结合高效液相色谱法测定水样中的甾体激素。

Determination of the steroid hormone levels in water samples by dispersive liquid-liquid microextraction with solidification of a floating organic drop followed by high-performance liquid chromatography.

机构信息

Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan.

出版信息

Anal Chim Acta. 2010 Mar 3;662(1):39-43. doi: 10.1016/j.aca.2010.01.003. Epub 2010 Jan 11.

Abstract

In this study, the steroid hormone levels in river and tap water samples were determined by using a novel dispersive liquid-liquid microextraction method based on the solidification of a floating organic drop (DLLME-SFO). Several parameters were optimized, including the type and volume of the extraction and dispersive solvents, extraction time, and salt effect. DLLME-SFO is a fast, cheap, and easy-to-use method for detecting trace levels of samples. Most importantly, this method uses less-toxic solvent. The correlation coefficient of the calibration curve was higher than 0.9991. The linear range was from 5 to 1000 microg L(-1). The spiked environmental water samples were analyzed using DLLME-SFO. The relative recoveries ranged from 87% to 116% for river water (which was spiked with 4 microg L(-1) for E1, 3 microg L(-1) for E2, 4 microg L(-1) for EE2 and 9 microg L(-1) for E3) and 89% to 102% for tap water (which was spiked with 6 microg L(-1) for E1, 5 microg L(-1) for E2, 6 microg L(-1) for EE2 and 10 microg L(-1) for E3). The detection limits of the method ranged from 0.8 to 2.7 microg L(-1) for spiked river water and 1.4 to 3.1 microg L(-1) for spiked tap water. The methods precision ranged from 8% to 14% for spiked river water and 7% to 14% for spiked tap water.

摘要

在这项研究中,采用基于悬浮有机液滴(DLLME-SFO)固化的新型分散液-液微萃取方法,测定了河水和自来水中的类固醇激素水平。优化了几个参数,包括萃取和分散溶剂的类型和体积、萃取时间和盐效应。DLLME-SFO 是一种快速、廉价且易于使用的方法,可用于检测痕量样品。最重要的是,这种方法使用毒性较小的溶剂。校准曲线的相关系数高于 0.9991。线性范围为 5 至 1000μg/L。使用 DLLME-SFO 分析了加标环境水样。河水(加标浓度为 E1 4μg/L、E2 3μg/L、EE2 4μg/L 和 E3 9μg/L)的相对回收率在 87%至 116%之间,自来水(加标浓度为 E1 6μg/L、E2 5μg/L、EE2 6μg/L 和 E3 10μg/L)的相对回收率在 89%至 102%之间。该方法的检出限为加标河水的 0.8 至 2.7μg/L 和加标自来水的 1.4 至 3.1μg/L。加标河水的方法精密度在 8%至 14%之间,加标自来水的方法精密度在 7%至 14%之间。

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