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基于浮质有机液滴固化的两种微萃取方法的比较,用于采用中心复合设计的液相色谱串联质谱法测定河水样品中的多类分析物。

Comparison of two microextraction methods based on solidification of floating organic droplet for the determination of multiclass analytes in river water samples by liquid chromatography tandem mass spectrometry using Central Composite Design.

作者信息

Asati Ankita, Satyanarayana G N V, Patel Devendra K

机构信息

Academy of Scientific & Innovative Research (AcSIR), CSIR-IITR campus, Lucknow, India; Analytical Chemistry Division and Regulatory Toxicology Group, CSIR-Indian Institute of Toxicology Research, Vishvigyan Bhawan 31, Mahatma Gandhi Marg, Lucknow-226001, U.P., India.

Analytical Chemistry Division and Regulatory Toxicology Group, CSIR-Indian Institute of Toxicology Research, Vishvigyan Bhawan 31, Mahatma Gandhi Marg, Lucknow-226001, U.P., India; Department of Chemistry, School of Applied Sciences, Babu Banarasi Das University, BBD City, Faizabad Road, Lucknow-226028, U.P., India.

出版信息

J Chromatogr A. 2017 Sep 1;1513:157-171. doi: 10.1016/j.chroma.2017.07.048. Epub 2017 Jul 15.

Abstract

Two low density organic solvents based liquid-liquid microextraction methods, namely Vortex assisted liquid-liquid microextraction based on solidification of floating organic droplet (VALLME-SFO) and Dispersive liquid-liquid microextraction based on solidification of floating organic droplet(DLLME-SFO) have been compared for the determination of multiclass analytes (pesticides, plasticizers, pharmaceuticals and personal care products) in river water samples by using liquid chromatography tandem mass spectrometry (LC-MS/MS). The effect of various experimental parameters on the efficiency of the two methods and their optimum values were studied with the aid of Central Composite Design (CCD) and Response Surface Methodology(RSM). Under optimal conditions, VALLME-SFO was validated in terms of limit of detection, limit of quantification, dynamic linearity range, determination of coefficient, enrichment factor and extraction recovery for which the respective values were (0.011-0.219ngmL), (0.035-0.723ngmL), (0.050-0.500ngmL), (R=0.992-0.999), (40-56), (80-106%). However, when the DLLME-SFO method was validated under optimal conditions, the range of values of limit of detection, limit of quantification, dynamic linearity range, determination of coefficient, enrichment factor and extraction recovery were (0.025-0.377ngmL), (0.083-1.256ngmL), (0.100-1.000ngmL), (R=0.990-0.999), (35-49), (69-98%) respectively. Interday and intraday precisions were calculated as percent relative standard deviation (%RSD) and the values were ≤15% for VALLME-SFO and DLLME-SFO methods. Both methods were successfully applied for determining multiclass analytes in river water samples.

摘要

本文比较了两种基于低密度有机溶剂的液-液微萃取方法,即基于漂浮有机液滴固化的涡旋辅助液-液微萃取(VALLME-SFO)和基于漂浮有机液滴固化的分散液-液微萃取(DLLME-SFO),采用液相色谱串联质谱法(LC-MS/MS)测定河水样品中的多类分析物(农药、增塑剂、药物和个人护理产品)。借助中心复合设计(CCD)和响应面方法(RSM)研究了各种实验参数对这两种方法效率的影响及其最佳值。在最佳条件下,对VALLME-SFO方法的检测限、定量限、动态线性范围、决定系数、富集因子和萃取回收率进行了验证,其各自的值分别为(0.011-0.219ng/mL)、(0.035-0.723ng/mL)、(0.050-0.500ng/mL)、(R=0.992-0.999)、(40-56)和(80-106%)。然而,当在最佳条件下对DLLME-SFO方法进行验证时,检测限、定量限、动态线性范围、决定系数、富集因子和萃取回收率的值范围分别为(0.025-0.377ng/mL)、(0.083-1.256ng/mL)、(0.100-1.000ng/mL)、(R=0.990-0.999)、(35-49)和(69-98%)。日间和日内精密度以相对标准偏差百分比(%RSD)计算,VALLME-SFO和DLLME-SFO方法的值均≤15%。两种方法均成功应用于测定河水样品中的多类分析物。

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