Chemical Derivatizations in Analytical Extractions

Rosenfeld, Jack

doi:10.1002/9780813823621.ch13

Cited by 8 publications

(3 citation statements)

References 213 publications

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“…2,7,216,217 Derivatization types of every kind have been utilized for detection of important environmental analytes. Given the variety of types of analytes, which fall under this category, and the multitude of techniques employed to analytically assess components, it is not reasonable to expect a common approach to derivatization methods.…”

Section: Environmentalmentioning

confidence: 99%

Analytical Derivatization Techniques ☆

Parkinson¹

2014

Reference Module in Chemistry, Molecular Sciences and Chemical Engineering

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For the last 40 years or so, analytical chemists have borrowed well-known reaction techniques from organic and organometallic fields to perform derivatization reactions so as to enhance detection of the elusive analytes they seek. The derivatization mantra has been that, for the technique to be worthwhile, it should be simple to perform, fast (usually less than 15 min), selective, and that the derivatizing reagent should react quantitatively with the analyte and only give one final product. So where are we now? Some derivatization reactions are indeed fast and some are not; some are very selective and some are more universal. However, with a certain care and careful control of optimized conditions, quantitative enhancement outcomes and increased separative power and detection can be very worthwhile. The number of derivatization reagents commercially available itself suggests that there must be some merit to derivatization, that overcomes the associated extra costs: in time (to incorporate the extra reaction step), and in the expense of acquiring, handling, and storing derivatizing reagents. This chapter attempts to show that with proper consideration, it has been feasible to push a chosen analytical technique to give increased selective detection and signal enhancement by derivatization. In many cases, this has made possible the detection of trace components from difficult matrices in a number of scenarios, including on-site analysis, in quality control/continuous analysis methods, or through some remote-sensing platforms. Further, the incorporation of derivatization in an extraction method can be simple and friendly to automated throughput for multiple sample analysis.The fundamental idea of derivatization is that the basic chemical or physical structure of the analytical moiety is changed through a suitable reaction. For example, by labeling compounds for a specific detection purpose, or by changing a functional group to enhance certain chromatographic characteristics, better detection and separation (respectively) can be achieved via the ensuing instrumental techniques. The type of derivatization is highly dependent upon the analytical method and upon the nature of the compound analyzed. There are a variety of good review articles, technical reports, 1 text chapters, 2 and full texts 3-6 that address in detail many specific applications used in analytical derivatization. There are several extraction methods available that are compatible with derivatization. For many analyses, the choice of the best extraction technique is not clear, as many techniques can extract analytes equally well, based on simplicity, applicability, solvent use, expense, detection limit, precision, and time taken to perform the operation. 7 Derivatization techniques have been incorporated into many sample preparation and extractions schemes, to include, but not limited to, total sample headspace, single-drop microextraction (SDME), 8 solid-phase microextraction (SPME), needle trap device (NTD), purge and trap, solid-phase extraction (SPE)...

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Section: Environmentalmentioning

confidence: 99%

Analytical Derivatization Techniques ☆

Parkinson¹

2014

Reference Module in Chemistry, Molecular Sciences and Chemical Engineering

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“…2,5 Thiols are difficult analytes to extract and quantitate, and there is a need to find a sampling and extraction technique that will allow thiol substitution differentiation while maintaining careful control of sampling and analysis conditions for quantitation. The technique of derivatization has been applied to many GC and GC-MS analysis techniques, 6,7 and a review of thiol derivatization 8 is informative. Derivatization offers a number of benefits that include higher temperature stability, improved analyte separation, and signal enhancement for derivatized components (often >100-fold) and hence allow lower detection limits of such compounds to be achieved and increase the working range for calibrative quantitation.…”

Section: ■ Introductionmentioning

confidence: 99%

“…The technique of derivatization has been applied to many GC and GC-MS analysis techniques, , and a review of thiol derivatization is informative. Derivatization offers a number of benefits that include higher temperature stability, improved analyte separation, and signal enhancement for derivatized components (often >100-fold) and hence allow lower detection limits of such compounds to be achieved and increase the working range for calibrative quantitation.…”

Section: Introductionmentioning

confidence: 99%

Assessment of Thiol Compounds from Garlic by Automated Headspace Derivatized In-Needle-NTD-GC-MS and Derivatized In-Fiber-SPME-GC-MS

Warren

Parkinson

Pawliszyn

2013

J. Agric. Food Chem.

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This study investigates the analysis of thiol compounds using a needle trap device (HS-NTD) and solid-phase microextraction (HS-SPME) derivatized headspace techniques coupled to GC-MS. Thiol compounds and their outgassed products are particularly difficult to monitor in foodstuffs. It was found that with in-needle and in-fiber derivatization, using the derivatization agent N-phenylmaleimide, it was possible to enhance the selectivity toward thiol, which allowed the quantitation of butanethiol, ethanethiol, methanethiol, and propanethiol compounds found in fresh garlic. A side-hole NTD was prepared and packed in house and utilized mixed DVB and Carboxen polymer extraction phases made of 60-80 mesh particles. NTD sampling was accomplished in the exhaustive sampling mode, where breakthrough was negligible. This work demonstrates a new application for a side-hole NTD sampling. A commercial mixed polymer phase of polydimethylsiloxane (PDMS) and divinylbenzene polymer (DVB) SPME fiber was used for SPME extractions. Under optimized derivatization, extraction, and analysis conditions for both NTD-GC-MS and SPME-GC-MS techniques, automated sampling methods were developed for quantitation. Both methods demonstrate a successful approach to thiol determination and provide a quantitative linear response between <0.1 and 10 mg L(-1) (R(2) = 0.9996), with limits of detection (LOD) in the low micrograms per liter range for the investigated thiols. Addition methods using known spiked quantities of thiol analytes in ground garlic facilitated method validation. Carry-over was also negligible for both SPME and NTD under optimized conditions.

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Principles of Analytical Chemistry for Toxicology

Durner

Watts

2021

Regulatory Toxicology

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Chemical Derivatizations in Analytical Extractions

Cited by 8 publications

References 213 publications

Analytical Derivatization Techniques ☆

Analytical Derivatization Techniques ☆

Assessment of Thiol Compounds from Garlic by Automated Headspace Derivatized In-Needle-NTD-GC-MS and Derivatized In-Fiber-SPME-GC-MS

Principles of Analytical Chemistry for Toxicology

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