Microextraction by Packed Sorbent (MEPS) and Solid-Phase Microextraction (SPME) as Sample Preparation Procedures for the Metabolomic Profiling of Urine

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.

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

Journal of Chemistry ◽

10.1155/2015/239016 ◽

2015 ◽

Vol 2015 ◽

pp. 1-9 ◽

Cited By ~ 1

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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Alternative sample preparation method for photochemical studies based on solid phase microextraction: Synthetic pyrethroid photochemistry

Journal of Chromatography A ◽

10.1016/j.chroma.2006.12.095 ◽

2007 ◽

Vol 1152 (1-2) ◽

pp. 156-167 ◽

Cited By ~ 24

Author(s):

M. Fernández-Álvarez ◽

L. Sánchez-Prado ◽

M. Lores ◽

M. Llompart ◽

C. García-Jares ◽

...

Keyword(s):

Sample Preparation ◽

Solid Phase Microextraction ◽

Preparation Method ◽

Solid Phase ◽

Synthetic Pyrethroid ◽

Sample Preparation Method

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

Reviews in Analytical Chemistry ◽

10.1515/revac-2017-0018 ◽

2018 ◽

Vol 37 (2) ◽

Cited By ~ 4

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.

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Chemometric Study and Optimization of Headspace Solid-Phase Microextraction Parameters for the Determination of Multiclass Pesticide Residues in Processed Cocoa from Nigeria Using Gas Chromatography/Mass Spectrometry

Journal of AOAC International ◽

10.5740/jaoacint.sgeabdulrauf ◽

2014 ◽

Vol 97 (4) ◽

pp. 1007-1011 ◽

Cited By ~ 6

Author(s):

Lukman Bola Abdulra'uf ◽

Guan Huat Tan

Keyword(s):

Sample Preparation ◽

Pesticide Residues ◽

Solid Phase Microextraction ◽

Solid Phase ◽

Internal Standard ◽

Calibration Method ◽

Gas Chromatography Mass Spectrometry ◽

Design Matrix ◽

Analytical Methodology ◽

Cocoa Powder

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%.

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An approach to solventless sample preparation procedure for pesticides analysis using solid phase microextraction/supercritical fluid extraction technique

Analytica Chimica Acta ◽

10.1016/s0003-2670(00)00944-2 ◽

2000 ◽

Vol 418 (1) ◽

pp. 69-77 ◽

Cited By ~ 24

Author(s):

Shamsul Hairi Salleh ◽

Yoshihiro Saito ◽

Kiyokatsu Jinno

Keyword(s):

Sample Preparation ◽

Supercritical Fluid Extraction ◽

Supercritical Fluid ◽

Solid Phase Microextraction ◽

Solid Phase ◽

Preparation Procedure ◽

Extraction Technique ◽

Fluid Extraction ◽

Sample Preparation Procedure

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Liquid–Solid Sample Preparation Followed by Headspace Solid-Phase Microextraction Determination of Multiclass Pesticides in Soil

Journal of AOAC International ◽

10.5740/jaoacint.sge_durovic ◽

2012 ◽

Vol 95 (5) ◽

pp. 1331-1337 ◽

Cited By ~ 7

Author(s):

Rada D Ðurović ◽

Tijana M Ðorðević ◽

Ljiljana R Šantrić

Keyword(s):

Sample Preparation ◽

Solid Phase Microextraction ◽

Solid Phase ◽

Extraction Procedure ◽

Soil Samples ◽

Optimum Number ◽

Headspace Solid Phase Microextraction ◽

Extraction Solvents ◽

Development And Validation

Abstract This paper describes development and validation of a multiresidue method for the determination of five pesticides (terbufos, prochloraz, chloridazon, pendimethalin, and fluorochloridone) belonging to different pesticide groups in soil samples by GC/MS, followed by its application in the analysis of some agricultural soil samples. The method is based on a headspace solid-phase microextraction method. Microextraction conditions, namely temperature, extraction time, and NaCl content, were tested and optimized using a 100 μm polydimethylsiloxane fiber. Three extraction solvents [methanol, methanol–acetone (1 + 1, v/v), and methanol–acetone–hexane (2 + 2 + 1, v/v/v)] and the optimum number of extraction steps within the sample preparation stage were optimized for the extraction procedure. LOD values for all the studied compounds were less than 12 μg/kg. Recovery values for multiple analyses of soil samples fortified at 30 μg/kg of each pesticide were higher than 64%. The method was proven to be repeatable, with RSD lower than 15%.

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