Electrochemically Fabricated Solid Phase Microextraction Fibers and Their Applications in Food, Environmental and Clinical Analysis

2019 ◽  
Vol 15 (7) ◽  
pp. 706-730 ◽  
Author(s):  
Levent Pelit ◽  
Füsun Pelit ◽  
Hasan Ertaş ◽  
Fatma Nil Ertaş
Keyword(s):  
Sample Preparation ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Clinical Analysis ◽  
Fine Tuning ◽  
Hazardous Substances ◽  
Preparation Technique ◽  
Vast Number ◽  
Electrochemical Preparation ◽  
Wide Range

Background:Designing an analytical methodology for complicated matrices, such as biological and environmental samples, is difficult since the sample preparation procedure is the most demanding step affecting the whole analytical process. Nowadays, this step has become more challenging by the legislations and environmental concerns since it is a prerequisite to eliminate or minimize the use of hazardous substances in traditional procedures by replacing with green techniques suitable for the sample matrix.Methods:In addition to the matrix, the nature of the analyte also influence the ease of creating green analytical techniques. Recent developments in the chemical analysis provide us new methodologies introducing microextraction techniques and among them, solid phase microextraction (SPME) has emerged as a simple, fast, low cost, reliable and portable sample preparation technique that minimizes solvent consumption.Results:The use of home-made fibers is popular in the last two decades since the selectivity can be tuned by changing the surface characteristics through chemical and electrochemical modifications. Latter technique is preferred since the electroactive polymers can be coated onto the fiber under controlled electrochemical conditions and the film thicknesses can be adjusted by simply changing the deposition parameters. Thermal resistance and mechanical strength can be readily increased by incorporating different dopant ions into the polymeric structure and selectivity can be tuned by inserting functional groups and nanostructures. A vast number of analytes with wide range of polarities extracted by this means can be determined with a suitable chromatographic detector coupled to the system. Therefore, the main task is to improve the physicochemical properties of the fiber along with the extraction efficiency and selectivity towards the various analytes by adjusting the electrochemical preparation conditions.Conclusion:This review covers the fine tuning conditions practiced in electrochemical preparation of SPME fibers and in-tube systems and their applications in environmental, food and clinical analysis.

scholarly journals Developments of solid-phase microextraction fiber coatings for environmental pharmaceutical and personal care products analysis

2018 ◽  
Vol 37 (2) ◽  
Author(s):  
Omar J. Portillo-Castillo ◽  
Rocío Castro-Ríos ◽  
Abelardo Chávez-Montes ◽  
Azucena González-Horta ◽  
Norma Cavazos-Rocha ◽  
...  
Keyword(s):  
Sample Preparation ◽  
Environmental Samples ◽  
Solid Phase Microextraction ◽  
Emerging Contaminants ◽  
Solid Phase ◽  
Personal Care Products ◽  
Preparation Technique ◽  
Personal Care ◽  
Promising Alternative ◽  
Monitoring Protocols

Abstract Solid-phase microextraction (SPME) is a sample preparation technique with many applications that is being continuously developed. In this technique, the type of fiber coating plays a crucial role for extraction efficiency. Currently available commercial coatings have certain drawbacks that have been overcome by the development of new coatings based on novel materials; these have improved the efficiency of extraction, selectivity and stability of commercial coatings. Pharmaceutical and personal care products (PPCPs) are one of the most important groups of emerging contaminants; however, some studies suggest that these compounds can cause adverse health effects. No official monitoring protocols for these compounds are currently available, so the establishment of analytical methods that allow their determination in environmental samples is required. The complexity of environmental samples together with the low concentration levels of these compounds makes necessary the use of sample preparation techniques capable of removing interferences, as well as preconcentrated analytes, and SPME is a very promising alternative to achieve this. This review describes the recent developments in SPME with classical and novel coatings and its applications for PPCP determination in environmental samples.

In situ Surfactant-based Solid Phase Microextraction of p-cresol in Human Plasma Prior to HPLC Analysis

2020 ◽  
Vol 16 (6) ◽  
pp. 687-694
Author(s):  
Azam Samadi ◽  
Abolghasem Jouyban ◽  
Negar Amirhaghiian ◽  
Hamid Tayebi-Khosroshahi
Keyword(s):  
Sample Preparation ◽  
Human Plasma ◽  
Solid Phase Microextraction ◽  
Hplc Analysis ◽  
Solid Phase ◽  
Uremic Toxin ◽  
Preparation Technique ◽  
Plasma Samples ◽  
Waste Products

Background:Uremia is the outcome of the remaining of nitrogenous waste products that are normally removed by the kidneys. Para-cresol (4-methylphenol) can be regarded as a proteinbound uremic toxin. The p-cresol determination in sera is necessary since it is a marker of cardiovascular risk and overall mortality in hemodialysis patients. Among the reported methods, chromatographic ones especially HPLC techniques due to the high sensitivity, selectivity and reproducibility have been extensively exploited in analysis of p-cresol in complex mixtures. However, an appropriate sample preparation prior to analysis is necessary for obtaining accurate and precise results.Methods:In this study, the appropriate precipitating agent for p-cresol determination in plasma samples was investigated. Then, in situ surfactant-based solid phase microextraction followed by HPLCFL detection was developed and validated for the quantification of p-cresol in plasma samples.Results:According to the results, HCl/heat precipitation method was used for p-cresol microextraction from from plasma samples. In situ surfactant-based solid phase microextraction using cetyltrimethylammonium bromide as extraction medium was proposed for pretreatment of plasma samples prior to analysis. The separation was achieved by isocratic elution with sodium acetate buffer (pH 3.8) and acetonitrile (20:80, v/v). Linearity was found to be acceptable over the concentration ranges of 0.5 to 8 μg mL-1 with the limit of detection and quantification of 0.324 and 0.422 μg mL-1, respectively. The variations for intra-day and inter-day precisions were both less than 8.2% and the extraction recoveries were more than 97%.Conclusion:A validated ISS-SPME followed by HPLC-FL detection reported to determine the total p-cresol concentration of human plasma samples. The traditional liquid-liquid extraction techniques are normally time consuming and require the use of large amounts of toxic organic solvents. In addition, the evaporation of extraction solvent and dissolving the analyte in the mobile phase is commonly used before HPLC analysis. Such a requirement makes the sample preparation process even more tedious and time consuming. ISS-SPME that is the developed ISS-SPE in micro scale, is a simple, rapid and effective sample preparation technique that is appropriate for HPLC-FL analysis.

scholarly journals Fabric Phase Sorptive Extraction: A Paradigm Shift Approach in Analytical and Bioanalytical Sample Preparation

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 865 ◽  
Author(s):  
Abuzar Kabir ◽  
Victoria Samanidou
Keyword(s):  
Sample Preparation ◽  
Anion Exchanger ◽  
Paradigm Shift ◽  
Mixed Mode ◽  
Cation Exchanger ◽  
Solid Phase ◽  
Sol Gel ◽  
Preparation Technique ◽  
Sorptive Extraction ◽  
Wide Range

Fabric phase sorptive extraction (FPSE) is an evolutionary sample preparation approach which was introduced in 2014, meeting all green analytical chemistry (GAC) requirements by implementing a natural or synthetic permeable and flexible fabric substrate to host a chemically coated sol–gel organic–inorganic hybrid sorbent in the form of an ultra-thin coating. This construction results in a versatile, fast, and sensitive micro-extraction device. The user-friendly FPSE membrane allows direct extraction of analytes with no sample modification, thus eliminating/minimizing the sample pre-treatment steps, which are not only time consuming, but are also considered the primary source of major analyte loss. Sol–gel sorbent-coated FPSE membranes possess high chemical, solvent, and thermal stability due to the strong covalent bonding between the fabric substrate and the sol–gel sorbent coating. Subsequent to the extraction on FPSE membrane, a wide range of organic solvents can be used in a small volume to exhaustively back-extract the analytes after FPSE process, leading to a high preconcentration factor. In most cases, no solvent evaporation and sample reconstitution are necessary. In addition to the extensive simplification of the sample preparation workflow, FPSE has also innovatively combined the extraction principle of two major, yet competing sample preparation techniques: solid phase extraction (SPE) with its characteristic exhaustive extraction, and solid phase microextraction (SPME) with its characteristic equilibrium driven extraction mechanism. Furthermore, FPSE has offered the most comprehensive cache of sorbent chemistry by successfully combining almost all of the sorbents traditionally used exclusively in either SPE or in SPME. FPSE is the first sample preparation technique to exploit the substrate surface chemistry that complements the overall selectivity and the extraction efficiency of the device. As such, FPSE indeed represents a paradigm shift approach in analytical/bioanalytical sample preparation. Furthermore, an FPSE membrane can be used as an SPME fiber or as an SPE disk for sample preparation, owing to its special geometric advantage. So far, FPSE has overwhelmingly attracted the interest of the separation scientist community, and many analytical scientists have been developing new methodologies by implementing this cutting-edge technique for the extraction and determination of many analytes at their trace and ultra-trace level concentrations in environmental samples as well as in food, pharmaceutical, and biological samples. FPSE offers a total sample preparation solution by providing neutral, cation exchanger, anion exchanger, mixed mode cation exchanger, mixed mode anion exchanger, zwitterionic, and mixed mode zwitterionic sorbents to deal with any analyte regardless of its polarity, ionic state, or the sample matrix where it resides. Herein we present the theoretical background, synthesis, mechanisms of extraction and desorption, the types of sorbents, and the main applications of FPSE so far according to different sample categories, and to briefly show the progress, advantages, and the main principles of the proposed technique.

scholarly journals Implementing Green Analytical Methodologies Using Solid-Phase Microextraction: A Review

Molecules ◽  
2020 ◽  
Vol 25 (22) ◽  
pp. 5297
Author(s):  
Kayla M. Billiard ◽  
Amanda R. Dershem ◽  
Emanuela Gionfriddo
Keyword(s):  
Analytical Chemistry ◽  
Sample Preparation ◽  
Analytical Method ◽  
Analytical Methods ◽  
Solid Phase Microextraction ◽  
Method Development ◽  
Assessment Tool ◽  
Solid Phase ◽  
Assessment Tools ◽  
Green Analytical Chemistry

Implementing green analytical methodologies has been one of the main objectives of the analytical chemistry community for the past two decades. Sample preparation and extraction procedures are two parts of analytical method development that can be best adapted to meet the principles of green analytical chemistry. The goal of transitioning to green analytical chemistry is to establish new methods that perform comparably—or superiorly—to traditional methods. The use of assessment tools to provide an objective and concise evaluation of the analytical methods’ adherence to the principles of green analytical chemistry is critical to achieving this goal. In this review, we describe various sample preparation and extraction methods that can be used to increase the greenness of a given analytical method. We gave special emphasis to modern microextraction technologies and their important contributions to the development of new green analytical methods. Several manuscripts in which the greenness of a solid-phase microextraction (SPME) technique was compared to other sample preparation strategies using the Green Analytical Procedure Index (GAPI), a green assessment tool, were reviewed.

scholarly journals Determination of Volatile Compounds in Foxtail Millet Sake Using Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry

2015 ◽  
Vol 2015 ◽  
pp. 1-9 ◽  
Author(s):  
Jingke Liu ◽  
Wei Zhao ◽  
Shaohui Li ◽  
Aixia Zhang ◽  
Yuzong Zhang ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Sample Preparation ◽  
Volatile Compounds ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Foxtail Millet ◽  
Diethyl Ester ◽  
Fiber Types ◽  
Headspace Solid Phase Microextraction ◽  
Spme Fiber

The volatile compounds in foxtail millet sake were extracted by headspace solid-phase microextraction (HS-SPME) and analyzed using gas chromatography-mass spectroscopy (GC-MS). Different methods of sample preparation were used to optimize this method (SPME fiber types, sample amount, extraction time, extraction temperature, content of NaCl, and rotor speed). For final method of sample preparation, 8 mL of sake was placed in a 15 mL headspace vial with addition of 1.5 g of NaCl; a 50/30 μm DVB/CAR/PDMS SPME fiber was used for extraction at 50°C for 30 min with 10 rpm continuous stirring. A total of 41 volatile compounds were identified from the sake sample, including 9 esters, 6 alcohols, 4 acids, 4 aldehydes, 9 hydrocarbons, 7 benzene derivatives, and 2 others. The main volatile compounds were ethyl acetate, phenylethyl alcohol, butanedioic acid diethyl ester, and hexadecane. According to their odors active values (OAVs), 10 volatile compounds were established to be odor active compounds and to contribute to the typical foxtail millet sake aroma. Hexanoic acid ethyl ester was the most prominent odor active compound.

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