scholarly journals Microfluidic Flow-through SPME Chip for Online Separation and MS Detection of Multiple Analyses in Complex Matrix

Micromachines ◽  
2020 ◽  
Vol 11 (2) ◽  
pp. 120
Author(s):  
Yujun Chen ◽  
Tao Gong ◽  
Cilong Yu ◽  
Xiang Qian ◽  
Xiaohao Wang

Simplifying tedious sample preparation procedures to improve analysis efficiency is a major challenge in contemporary analytical chemistry. Solid phase microextraction (SPME), a technology developed for rapid sample pretreatment, has flexibility in design, geometry, and calibration strategies, which makes it a useful tool in a variety of fields, especially environmental and life sciences. Therefore, it is important to study the coupling between the microfluidic electrospray ionization (ESI) chip integrated with the solid phase microextraction (SPME) module and the electrospray mass spectrometer (MS). In our previous work, we designed a solid phase microextraction (SPME) module on a microfluidic chip through geometric design. However, automation and calibration methods for the extraction process remain unresolved in the SPME on-chip domain, which will lead to faster and more accurate results. This paper discusses the necessity to design a micromixer structure that can produce different elution conditions on the microfluidic chip. By calculating the channel resistances, the microfluidic chip’s integrated module with the micromixer, SPME, and ESI emitters optimize the geometry structure. We propose the annular channel for SPME to perform the resistances balance of the entire chip. Finally, for SPME on a single chip, this work provides a quantitation calibration method to describe the distribution of the analytes between the sample and the extraction phase before reaching the adsorption equilibrium.

2014 ◽  
Vol 97 (4) ◽  
pp. 1007-1011 ◽  
Author(s):  
Lukman Bola Abdulra'uf ◽  
Guan Huat Tan

Abstract Solid-phase microextraction (SPME) is a solventless sample preparation method that combines sample preparation, isolation, concentration, and enrichment into one step. A simple and effective method coupling headspace-SPME to GC/MS was developed for the analysis of chlorpyrifos, fenitrothion, endosulfan I, and endosulfan II pesticide residues in cocoa powder. In this study, multivariate strategy was used to determine the significance of the factors affecting the SPME of the pesticides using a Plackett-Burman design, and the significant factors were optimized using central composite design. The analytes were extracted with 100 μm polydimethylsiloxane fibers according to the factorial design matrix and desorbed into a GC/MS instrument. The developed method was applied for the analysis of a cocoa powder sample, and it exhibited good figures of merit for the analytical methodology. Using the optimized conditions, the linearity ranged from 2.5 to 500 μg/kg (R2 > 0.99) using an internal standard calibration method, and the average recoveries were between 75 and 95%, with RSD values between 3.8 and 9.7%.


Author(s):  
Abookleesh L Frage , Almrhag M. Omar , Zatout M. Massoud

Headspace solid phase microextraction, fundamental& principle with its application on the determination of various pesticides are reviewed in this article. Pesticides extraction as a sample preparation step prior to subsequent analysis is aimed to achieve a reliable and accurate determination of this contaminants residue in food. Fast and high efficiency extraction process with free solvent consumption and overall cost is achieved through headspace solid phase micro extraction. HSPME is an equilibrium process which depends on the physio-chemical properties of the analyte to be extracted. Sample preparation and extraction condition such as fiber coating, temperature, time etc, have a direct impact on the extraction efficiency and sensitivity of headspace technique.


2015 ◽  
Vol 3 (1) ◽  
pp. 31
Author(s):  
Dwinna Rahmi

 ABSTRACT A syringe-based sample pretreatment tool, named herein “chelating monolith”, has been developed for simple and facile solid phase microextraction (SPME) of trace elements in natural waters. The monolith was directly prepared within the confines of a commercially available syringe filter tip by a two-step process: 1) in situ polymerization of glycidyl methacrylate (GMA) with ethylene glycol dimethacrylate (EDMA) and 2) subsequent modification with iminodiacetate (IDA) via ring opening reaction of epoxide. The composition of porogenic solvent was first optimized to make a rigid-porous material that has high permeability and ample surface area as much as possible. Then, the pH and concentration of the IDA modification solution were examined to obtain higher chelating capacity. The metal adsorption properties of the obtained chelating monolith were evaluated through an adsorption/desorption experiment. After optimization of some parameters such as sample solution pH, eluent concentration and the volume, good recoveries of more than 80% were obtained for 28 elements including REEs, Fe, Co, Ni, Cu, Zn, Ga, Pb and Th in a single extraction step. The proposed SPME method was validated through the analysis of river water certified reference material (CRM: JSAC 0301-1) Keywords: Solid phase microextraction; syringe filter; chelating monolith; iminodiacetate; ICP-MS


2012 ◽  
Vol 113 (3) ◽  
pp. 1667-1685 ◽  
Author(s):  
Agata Spietelun ◽  
Adam Kloskowski ◽  
Wojciech Chrzanowski ◽  
Jacek Namieśnik

Micromachines ◽  
2020 ◽  
Vol 11 (3) ◽  
pp. 285 ◽  
Author(s):  
Naresh Yandrapalli ◽  
Tina Seemann ◽  
Tom Robinson

Liposomes and giant unilamellar vesicles (GUVs) in particular are excellent compartments for constructing artificial cells. Traditionally, their use requires bench-top vesicle growth, followed by experimentation under a microscope. Such steps are time-consuming and can lead to loss of vesicles when they are transferred to an observation chamber. To overcome these issues, we present an integrated microfluidic chip which combines GUV formation, trapping, and multiple separate experiments in the same device. First, we optimized the buffer conditions to maximize both the yield and the subsequent trapping of the vesicles in micro-posts. Captured GUVs were monodisperse with specific size of 18 ± 4 µm in diameter. Next, we introduce a two-layer design with integrated valves which allows fast solution exchange in less than 20 s and on separate sub-populations of the trapped vesicles. We demonstrate that multiple experiments can be performed in a single chip with both membrane transport and permeabilization assays. In conclusion, we have developed a versatile all-in-one microfluidic chip with capabilities to produce and perform multiple experiments on a single batch of vesicles using low sample volumes. We expect this device will be highly advantageous for bottom-up synthetic biology where rapid encapsulation and visualization is required for enzymatic reactions.


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