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基于多变量实验设计优化的超声辅助和预富集,分散固相和分散液液微萃取结合分光光度法测定水样中孔雀石绿的比较。

Comparison between dispersive solid-phase and dispersive liquid-liquid microextraction combined with spectrophotometric determination of malachite green in water samples based on ultrasound-assisted and preconcentration under multi-variable experimental design optimization.

作者信息

Alipanahpour Dil Ebrahim, Ghaedi Mehrorang, Asfaram Arash, Zare Fahimeh, Mehrabi Fatemeh, Sadeghfar Fardin

机构信息

Young Researchers and Elite Club, Gachsaran Branch, Islamic Azad University, Gachsaran, Iran.

Chemistry Department, Yasouj University, Yasouj 75918-74831, Iran.

出版信息

Ultrason Sonochem. 2017 Nov;39:374-383. doi: 10.1016/j.ultsonch.2017.05.011. Epub 2017 May 8.

DOI:10.1016/j.ultsonch.2017.05.011
PMID:28732958
Abstract

The ultrasound-assisted dispersive solid-phase microextraction (USA-DSPME) and the ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME) developed for as an ultra preconcentration and/or technique for the determination of malachite green (MG) in water samples. Central composite design based on analysis of variance and desirability function guide finding best operational conditions and represent dependency of response to variables viz. volume of extraction, eluent and disperser solvent, pH, adsorbent mass and ultrasonication time has significant influence on methods efficiency. Optimum conditions was set for USA-DSPME as: 1mg CNTs/Zn:ZnO@NiP-NCs; 4min sonication time and 130μL eluent at pH 6.0. Meanwhile optimum point for USA-DLLME conditions were fixed at pH 6.0; 4min sonication time and 130, 650μL and 10mL of extraction solvent (CHCl), disperser solvent (ethanol) and sample volume, respectively. Under the above specified best operational conditions, the enrichment factors for the USA-DSPME and USA-DLLME were 88.89 and 147.30, respectively. The methods has linear response in the range of 20.0 to 4000.0ngmL with the correlation coefficients (r) between 0.9980 to 0.9995, while its reasonable detection limits viz. 1.386 to 2.348ngmL and good relative standard deviations varied from 1.1% to 2.8% (n=10) candidate this method for successful monitoring of analyte from various media. The relative recoveries of the MG dye from water samples at spiking level of 500ngmL were in the range between 94.50% and 98.86%. The proposed methods has been successfully applied to the analysis of the MG dye in water samples, and a satisfactory result was obtained.

摘要

为水样中孔雀石绿(MG)的测定开发了超声辅助分散固相微萃取(USA - DSPME)和超声辅助分散液液微萃取(USA - DLLME)作为超富集和/或技术。基于方差分析和期望函数的中心复合设计指导寻找最佳操作条件,并表示响应与变量(即萃取、洗脱剂和分散剂溶剂的体积、pH值、吸附剂质量和超声时间)之间的依赖性,对方法效率有显著影响。USA - DSPME的最佳条件设定为:1mg碳纳米管/锌:ZnO@NiP - NCs;超声时间4分钟,pH值6.0时洗脱剂为130μL。同时,USA - DLLME条件的最佳点固定在pH值6.0;超声时间4分钟,萃取溶剂(CHCl)、分散剂溶剂(乙醇)和样品体积分别为130、650μL和10mL。在上述指定的最佳操作条件下,USA - DSPME和USA - DLLME的富集因子分别为88.89和147.30。该方法在20.0至4000.0ng/mL范围内具有线性响应,相关系数(r)在0.9980至0.9995之间,其合理的检测限为1.386至2.348ng/mL,良好的相对标准偏差在1.1%至2.8%之间(n = 10),表明该方法可成功监测各种介质中的分析物。在500ng/mL加标水平下,水样中MG染料的相对回收率在94.50%至98.86%之间。所提出的方法已成功应用于水样中MG染料的分析,并获得了满意的结果。

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