Chapter 19 Recent developments in the chemistry and application of analytical derivatizations

Rosenfeld, Jack

doi:10.1016/s0166-526x(02)80056-3

Cited by 3 publications

(1 citation statement)

References 201 publications

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“…Extraction Combined with Derivatization. The selectivity and capacity of the extraction phase for analytes such as polar or ionic species, which are difficult to extract, can be frequently enhanced by introducing a derivatization step . The objective of derivatization is not only to convert the native analytes into less polar derivatives that are extracted more efficiently but also to label them for better detection or chromatography.…”

Section: Kineticsmentioning

confidence: 99%

Sample Preparation: Quo Vadis?

2003

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The sample preparation step in an analytical process typically consists of an extraction procedure that results in the isolation and enrichment of components of interest from a sample matrix. Extraction can vary in degree of selectivity, speed, and convenience and depends not only on the approach and conditions used but on the geometric configurations of the extraction phase. Increased interest in sample preparation research has been generated by the introduction of nontraditional extraction technologies. These technologies address the need for reduction of solvent use, automation, and miniaturization and ultimately lead to on-site in situ and in vivo implementation. These extraction approaches are frequently easier to operate but provide optimization challenges. More fundamental knowledge is required by an analytical chemist not only about equilibrium conditions but, more importantly, about the kinetics of mass transfer in the extraction systems. Optimization of this extraction process enhances overall analysis. Proper design of the extraction devices and procedures facilitates convenient on-site implementation, integration with sampling, and separation/quantification, automation, or both. The key to rational choice, optimization, and design is an understanding of the fundamental principles governing mass transfer of analytes in multiphase systems. The objective of this perspective is to summarize the fundamental aspects of sample preparation and anticipate future developments and research needs.

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Section: Kineticsmentioning

confidence: 99%

Sample Preparation: Quo Vadis?

2003

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Chemical Derivatizations in Analytical Extractions

Rosenfeld

2010

Handbook of Sample Preparation

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Development of an Impregnated Reagent and Automation of Solid-Phase Analytical Derivatization for Carbonyls: Proof of Principle

Rosenfeld

Kim

Rullo

2006

Journal of Chromatographic Science

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This study undertakes reduction of scale and automation of a solid-phase analytical derivatization of carbonyls with 2,4-dinitrophenylhyrazine on a styrene-divinylbenzene resin (XAD-2). Three processes are tested. In the batch process, an aqueous phase consisting of 50 microL of sample and 150 microL of reagent solution is contacted with 6 mg XAD-2 by shaking. An impregnated reagent consisting of 2,4-dinitrophenylhydrazine hydrochloride (DNPH) deposited on XAD-2 enables two additional processes. In-vial derivatization with an impregnated reagent requires shaking 50 microL of sample with 6 mg of the impregnated reagent and reduced the reaction time from 10 to 5 min. The third process involves packing impregnated reagent a mini-column and flowing 50 microL of sample through under positive pressure supplied by a Harvard Pump. This reduces sample preparation time to 1 min. Studies are conducted with worst-case model analytes: butanone, 2-pentanone, and malonyldialdehyde. The carbonyl of the two ketones is hindered, and, thus, these two compounds react very slowly with DNPH in aqueous solution. Malonyldialdehyde is highly water soluble, and it does not react in aqueous phase but also would not sorb onto XAD-2 for reaction. Nevertheless, derivatization/extraction of all model compounds any of the three procedures result in reproducible and high yields.

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Chapter 19 Recent developments in the chemistry and application of analytical derivatizations

Cited by 3 publications

References 201 publications

Sample Preparation: Quo Vadis?

Sample Preparation: Quo Vadis?

Chemical Derivatizations in Analytical Extractions

Development of an Impregnated Reagent and Automation of Solid-Phase Analytical Derivatization for Carbonyls: Proof of Principle

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