In-Vial Temperature Gradient Headspace Single Drop Microextraction Designed by Multiphysics Simulation
In-Vial Temperature Gradient Headspace Single Drop Microextraction Designed by Multiphysics Simulation
复制标题
通过多物理场模拟设计的瓶内温度梯度顶空单滴微萃取
DOI：
10.1021/acs.analchem.6b02514
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发表时间：
2016
影响因子：
7.4
通讯作者：
Cao Chengxi
中科院分区：
文献类型：
--
作者：
Jahan Sharmin;Zhang Qiang;Pratush Amit;Xie Haiyang;Xiao Hua;Fan Liuyin;Cao Chengxi
本文提出了一种基于温度梯度的顶空单滴微萃取（HS-SDME）技术，用于挥发性和半挥发性样品的现场预富集。首先，设计了一个内瓶盖作为HS-SDME单元中受体液滴的冷却装置，以实现快速高效的微萃取。第二，对于TG-HS-SDME，首次在80 °C的样品瓶中的供体相和在-20 °C的含有冷却液的内瓶盖下的受体液滴之间产生瓶内TG。第三，通过使用流体中的传热、Navier-Stokes方程和质量平衡方程进行条件优化以及基于COMSOL Multiphysics的动态照明，开发了一个简单的数学模型和数值模拟。选择5种氯酚类化合物作为模型化合物，对所提出的方法进行验证。结果表明，数值模拟结果与定量实验结果吻合较好，验证了TG-HS-SDME的设计。在最佳条件下，萃取富集提高了302- 388倍，仅在2分钟内，提供3.5至4倍的富集因子相比，一个典型的HS-SDME。模拟结果表明，这些改进的提取动力学可以归因于之间的样品基质和受体液滴的小体积的顶部空间内的应用温度差距。该方法线性范围为0.03 ~ 100 μg/L，相关系数R2> 0.9986，检出限为7-10 ng/L，重复性好（RSD <5.9%，n= 6）。所有的模拟和实验结果表明的鲁棒性，精度和实用性的TG-HS-SDME痕量分析的分析物在各种环境，制药，食品安全和法医样品。
Presented herein is a novel headspace single drop microextraction (HS-SDME) based on temperature gradient (TG) for an on-site preconcentration technique of volatile and semivolatile samples. First, an inner vial cap was designed as a cooling device for acceptor droplet in HS-SDME unit to achieve fast and efficient microextraction. Second, for the first time, an in-vial TG was generated between the donor phase in a sample vial at 80 °C and the acceptor droplet under the inner vial cap containing cooling liquid at −20 °C for a TG-HS-SDME. Third, a simple mathematic model and numerical simulations were developed by using heat transfer in fluids, Navier–Stokes and mass balance equations for conditional optimization, and dynamic illumination of the proposed extraction based on COMSOL Multiphysics. Five chlorophenols (CPs) were selected as model analytes to authenticate the proposed method. The comparisons revealed that the simulative results were in good agreement with the quantitative experiments, verifying the design of TG-HS-SDME via the numerical simulation. Under the optimum conditions, the extraction enrichments were improved from 302- to 388-fold within 2 min only, providing 3.5 to 4 times higher enrichment factors as compared to a typical HS-SDME. The simulation indicated that these improvements in the extraction kinetics could be attributed due to the applied temperature gap between the sample matrix and acceptor droplet within the small volume of headspace. Additionally, the experiments demonstrated a good linearity (0.03–100 μg/L,R2> 0.9986), low limit of detection (7–10 ng/L), and fair repeatability (<5.9% RSD,n= 6). All of the simulative and experimental results indicated the robustness, precision, and usefulness of TG-HS-SDME for trace analyses of analytes in a wide variety of environmental, pharmaceutical, food safety, and forensic samples.