Modern Sample Preparation for Chromatography

Modern Sample Preparation for Chromatography

2nd Edition - February 24, 2021

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  • Authors: Serban Moldoveanu, Victor David
  • Paperback ISBN: 9780128214053
  • eBook ISBN: 9780323898201

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Modern Sample Preparation for Chromatography, Second Edition explains the principles of sample preparation for chromatographic analysis. A variety of procedures are applied to make real-world samples amenable for chromatographic analysis and to improve results. This book's authors discuss each procedure’s advantages, disadvantages and their applicability to different types of samples, along with their fit for different types of chromatographic analysis. The book contains numerous literature references and examples of sample preparation for different matrices and new sections on green approaches in sample preparation, progress in automation of sample preparation, non-conventional solvents for LLE (ionic liquids, deep eutectic mixtures, and others), and more.

Key Features

  • Presents numerous techniques applied for sample preparation for chromatographic analysis
  • Provides an up-to-date source of information regarding the progress made in sample preparation for chromatography
  • Describes examples for specific types of matrices, providing a guide for choosing the appropriate sample preparation method for a given analysis


Analytical chemists involved in separation science; chemists of a wide range of levels from industry, research and academic sectors. Post-graduate and upper undergraduate students in analytical chemistry

Table of Contents

  • Part 1 - General concepts in sample preparation

    CHAPTER 1. Preliminaries to sample preparation

    1.1 Collection of information and planning for a chromatographic analysis

    General comments

    Flow of typical sampling and sample preparation process

    Chromatographic core analysis

    Collection of information regarding the analysis

    Planning the analysis

    Chemicals and certified reference materials

    References 1.4

    1.2 Statistical evaluation of quantitative data

    General aspects

    Precision and accuracy in quantitative chemical analysis

    Sensitivity and limit of detection

    Least square regression and linearity of the instrumental response

    Propagation of uncertainty

    Comparison of two procedures regarding accuracy

    Comparison of two procedures regarding precision

    Evaluation of the experimental design in sample preparation

    References 1.2

    1.3 Validation of an analytical method

    General aspects

    Validation procedures

    Parameters for method validation

    Acceptance criteria for validation

    References 1.3

    1.4 Sampling General comments

    Sampling procedures

    Some theoretical aspects of sampling

    Brief comments on sampling of gases

    Brief comments on sampling of liquids

    Brief comments on sampling of solids

    Brief comments on sampling of mixed-phases materials

    Some comments on sampling of biological materials

    Comments on handling, preservation, and storage of samples

    References 1.4


    CHAPTER 2. The role of sample preparation

    2.1 Preliminary processing of the sample

    General comments

    Sample homogenization

    Adjustment of water content in samples (drying)

    Sample dissolution

    Resampling for further reduction of sample size

    Green approaches in sample preparation

    References 2.2

    2.2 Routine manipulations of the sample

    General comments


    Volume measuring

    Mixing and dilution

    Heating and cooling

    Other routine sample manipulation

    Preservation of sample integrity during processing

    References 2.1

    2.3 Sample cleanup and fractionation

    General comments

    Cleanup and fractionation procedures

    Analyte recovery during sample cleanup

    References 2.3.

    2.4 Concentration of the sample

    General comments

    Enrichment factor

    References 2.4

    2.5 Chemical modifications of the sample

    General comments

    Chemical changes for sample dissolution

    Chemical changes for cleanup and fractionation purposes

    Chemical modification for the enhancement of detection

    Chemical modification for enhancing the separation in core chromatography

    References 2.5

    2.6 Selection of a sample preparation procedure

    General comments

    Development of a sample preparation scheme based on preliminary information

    "Dilute and shoot" in chromatographic analysis

    References 2.6

    2.7 Automation and high throughput in sample preparation

    General comments

    Off-line automation and sample preparation

    On-line automation and sample preparation

    Software controlling automation in sample preparation

    High-throughput sample preparation

    References 2.7

    CHAPTER 3. Chromatography as a core step for an analytical procedure

    3.1 Basic concepts in chromatography

    General comments

    Common types of chromatography

    Basic characterization of a chromatographic process

    Qualitative chromatographic analysis

    Quantitative chromatographic analysis

    Selection of the internal standards in chromatographic analysis

    The matrix effects in chromatography

    Effect of medium (solvent) used for sample injection

    References 3.1

    3.2 Overview of gas chromatography

    Retention and separation mechanism in gas chromatography

    Typical GC instrumentation

    Injection and injection port of a GC

    The oven of a gas chromatograph

    Chromatographic columns

    Detectors in gas chromatography

    The need for sample preparation in GC

    References 3.2

    3.3 Overview of high performance liquid chromatography

    Retention and separation mechanism in liquid chromatography

    Typical HPLC instrumentation

    Solvent supply and pumping system

    Mobile phase in HPLC


    Chromatographic column

    Detectors in HPLC

    The need for sample preparation in HPLC

    References 3.3

    3.4 Other chromatography types used as core analytical method

    General comments

    References 3.4.

    Part 2 - Main sample preparation techniques

    CHAPTER 4. Mechanical processing in sample preparation

    4.1 Grinding and sieving

    General comments

    Particle size reduction


    References 4.1

    4.2 Filtration, microfiltration, and ultrafiltration

    General aspects

    Theory of filtration of solids from liquids

    Filters and membranes properties

    Filters and membranes materials

    Filtering devices in the laboratory

    Continuous filtration

    In-vivo application of ultrafiltration

    References 4.2

    4.3 Centrifugation

    General aspects

    The use of centrifugation in connection with filtration and ultrafiltration

    References 4.3

    CHAPTER 5. Phase transfer in sample preparation

    5.1 Distillation, vaporization, and drying

    General comments

    Boiling point of liquids

    Theory of gas-liquid equilibrium for two-component systems

    Dependence of boiling point on pressure


    Distillation under vacuum plus centrifugal force

    Steam distillation and other distillation processes


    Drying and freeze-drying


    References 5.1

    5.2 Physical dissolution, crystallization, and precipitation

    General comments

    Dissolution process (physical dissolution) in sample preparation

    Solvents used in sample preparations

    Hildebrand solubility parameter

    Solubility based on octanol/water partition coefficient

    Rate of dissolution

    Solubility of ionic compounds

    Selection of sample solvent for injecting in a chromatographic instrument

    Crystallization and precipitation

    References 5.2

    CHAPTER 6. Solvent extraction

    6.1 Properties of solvents relevant in the extraction process

    General comments

    Solvent density, viscosity, and diffusion coefficient

    Superficial tension

    Dielectric constant, dipole moment, and polarizability

    Hydrogen bonding of solvent molecules

    Miscibility of solvents

    Solvent characterization based on octanol/water partition coefficient

    Solvent characterization based on liquid-gas partition

    Solvent characterization based on solvatochromic model and Kamlet-Taft parameters

    Solvent characterization based on other parameters

    References 6.1

    6.2 Conventional liquid-liquid extraction

    General comments

    Liquid-liquid partition equilibrium

    Distribution coefficient

    Partition equilibrium for ionic species, metal complexes, and ion pairs

    Elementary thermodynamic theory for solvent extraction

    Common liquid-liquid extraction procedures

    Quantitation when LLE is part of sample preparation

    Selection of solvents for the extraction process

    The influence of pH on extraction

    Chemical modifications that affect extraction

    Non-chemical factors affecting extraction Separation using liquid-liquid extraction

    References 6.2

    6.3 Special liquid-liquid extraction procedures

    General comments

    Single drop-phase microextraction (SDME)

    Membrane-assisted solvent extraction (MASE)

    Microporous membrane liquid-liquid extraction (MMLLE)

    Hollow fiber liquid phase microextraction (HF-LPME)

    Mass transfer in LPME

    Liquid-liquid-liquid-microextraction (LLLME)

    Dispersive liquid-liquid microextraction (DLLME)

    Salting-out assisted LLE (SALLE)

    Liquid-liquid extraction with low temperature partitioning

    Cloud-point extraction (CPE)

    Electrochemically-modulated LLE

    Simultaneous distillation and extraction

    Other LLE variants

    Automation in LLE

    References 6.3

    6.4 Conventional liquid-solid extraction

    General comments

    The rate of extraction in LSE

    Solvents used in SLE

    Simple extraction conditions

    Soxhlet extraction

    Separation using liquid-solid extraction

    References 6.4

    6.5 Accelerated solvent extraction

    General comments

    Instrumentation in ASE

    Selection of parameters for ASE operations Pressurized hot water extraction (PHWE)

    References 6.5

    6.6 Microwave assisted solvent extraction (MASE) and ultrasound assisted extraction (UAE)

    General comments

    Theory of microwave usage

    Practice of microwave extraction

    Development of other related MASE techniques

    Ultrasound assisted extraction

    References 6.6

    6.7 Supercritical solvent extraction

    General aspects

    Elementary theory of SFE extraction

    Diffusion coefficients for supercritical fluids

    Efficiency and selectivity in SFE

    Steps in the SFE process

    Optimization of the extraction

    Expansion of fluid and collection process in SFE

    SFE on-line with other chromatographic techniques

    References 6.7

    6.8 Solvent-gas extraction

    General aspects

    Headspace single-drop microextraction (HS-SDME)

    References 6.8

    CHAPTER 7. Solid-phase extraction

    7.1 Conventional solid-phase extraction

    General comments

    Practice of conventional solid-phase extraction

    Quantitation with a chromatographic method when SPE is part of sample preparation

    Equilibrium in solid-phase extraction

    Comparison of SPE with liquid chromatography

    Breakthrough volume in SPE

    References 7.1

    7.2 Chemical nature of materials used as SPE sorbent and their characterization

    General comments

    Inorganic porous materials

    Inorganic porous materials with an organic bonded surface

    Organic synthetic polymers

    Organic natural polymers

    Metal organic frameworks (MOFs) and covalent organic frameworks

    Magnetic nanoparticle sorbents

    Other materials used as SPE sorbents


    Physical properties of materials used as SPE sorbent

    Parameters characterizing SPE performance

    References 7.2

    7.3 Types of SPE sorbents according to their functionalities or function

    General comments

    Non-polar and weak polar SPE sorbents

    Polar SPE sorbents

    Ion exchange SPE sorbents

    Chelating ion exchange resins

    Affinity, immunoaffinity and aptamer sorbents

    Molecular imprinted polymers

    Restricted access media

    Mixed-mode sorbents

    Moisture and particulate removal SPE


    Other types of conventional sorbents used for SPE

    Monolithic materials

    Electrospun nanofibers


    Novelty sorbents

    References 7.3

    7.4 Formats used in SPE

    General comments

    Design and characteristics

    References 7.4

    7.5 Retention and elution mechanisms in SPE

    General comments

    Retention and elution on hydrophobic phases

    Retention and elution on polar phases

    Retention and elution on ion exchange phases

    References 7.5

    7.6 Solvents used in solid-phase extraction

    General comments

    Sorbent conditioning

    Selection of solvent for solute retention

    Selection of solvent for solute elution

    References 7.6

    7.7 Selection and optimization of solid-phase extraction

    Making the sample amenable for SPE

    Optimization of sorbents and solvents selection

    References 7.7

    7.8 Solid-phase extraction from headspace

    General aspects

    Sorbents used in headspace analysis

    Basic theory of static headspace extraction

    Practice of static headspace analysis

    Basic theory of dynamic headspace extraction

    Practice of dynamic headspace analysis

    Desorption of the analytes from the trap

    Purge and trap procedures

    Quantitation in headspace techniques

    Open tubular trapping

    References 7.8

    7.9 Solid-phase microextraction (SPME)

    General comments

    Basic theory of the retention of analytes on SPME fiber

    Common coatings for SPME fibers

    Other SPME coatings

    Desorption of analytes and conditioning of the SPME fiber

    Optimization of SPME analysis

    Qualitative and quantitative analysis with SPME

    Novel alternatives to the use of SPME

    On fiber derivatization in SPME

    SPME automation

    References 7.9

    7.10 Stir-bar sorptive extraction (SBSE)

    General comments

    Practice of SBSE

    Sorptive phase in SBSE

    Theory of SBSE

    References 7.10

    7.11 Matrix solid-phase dispersion (MSPD)

    Basic principle of MSPD

    Certain details on MSPD technique

    References 7.11

    7.12 QuEChERS technique

    General comments

    Steps of a QuEChERS procedure

    References 7.12

    CHAPTER 8. Chromatographic procedures as preliminary separations

    8.1 Thin layer and open column liquid chromatography as sample preparation

    General comments

    Thin layer chromatography as sample preparation

    Open (large) column liquid chromatography as sample preparation

    References 8.1

    8.2 Size exclusion chromatography (HPLC-SEC) used in sample preparation

    General comments about size exclusion

    Short theoretical background of SEC separation

    Stationary phases used in SEC

    Use of SEC as a sample preparation procedure

    References 8.2

    8.3 Other chromatographic techniques used for sample preparation

    General comments

    Flash chromatography

    Counter current chromatography

    References 8.3

    CHAPTER 9. Membrane separations as sample preparation techniques

    9.1 Gas diffusion through membranes

    General comments

    Basic theory of gas diffusion

    Utilization of gas diffusion through membranes as sample preparation

    References 9.1

    9.2 Membranes used in special liquid-liquid extraction

    General comments

    References 9.2

    9.3 Reversed osmosis and dialysis

    General comments

    Reverse osmosis


    Ion exchange membranes

    References 9.3

    CHAPTER 10. Electroseparations in sample preparation

    10.1 Electrophoretic techniques

    General comments

    Theoretical aspects of electrophoretic separations

    Electrophoretic techniques

    References 10.1

    10.2 Other electroseparation techniques

    General comments

    Electro-membrane LLE

    References 10.1

    CHAPTER 11. Other separation techniques in sample preparation

    11.1 Overview of ion exchange use in sample preparation

    General comments

    Applications of ion exchangers in sample preparation

    References 11.1

    11.2 Other techniques in sample preparation

    General comments

    Examples of applications as sample preparation for chromatography

    References 11.2

    CHAPTER 12. The role of derivatization in chromatography

    12.1 Derivatization for sample dissolution

    General comments

    Sample dissolution by pH change

    Other common dissolution procedures using chemical reactions

    References 12.1

    12.2 Improvement of gas chromatographic analysis by derivatization

    General comments

    Procedures for performing derivatization for gas chromatography

    Derivatization for making polar and/or nonvolatile compounds amenable for GC

    The role of derivatization in the improvement of separation

    Derivatization for improving sensitivity of detection

    Derivatization for improving compound identification

    Improvement of quantitation accuracy through derivatization

    References 12.2

    12.3 Improvement of liquid chromatographic analysis by derivatization

    General comments

    Procedures for performing derivatization for liquid chromatography

    The role of derivatization in the improvement of separation

    The role of derivatization in the improvement of detection sensitivity

    Improvement of quantitation accuracy through derivatization

    Derivatization for the improvement of stability of the analyte

    References 12.3

    12.4 Derivatization for chiral separations

    General comments

    Chromatographic chiral separations

    Derivatization with non-chiral (achiral) reagents

    Diastereoisomers generated by derivatization with chiral reagents

    References 12.4

    CHAPTER 13. Chemical reactions used in analytical derivatizations

    13.1 Reactions with formation of alkyl or aryl derivatives

    General comments

    Alkylation and arylation mechanisms Common alkylation reagents

    Artifact formation in alkylation reactions

    References 13.1

    13.2 Reactions with formation of silyl derivatives

    General comments

    Some aspects of silylation mechanism

    Reagents used for silylation

    Silylation for the introduction of groups other than TMS

    Artifact formation in trimethylsilyl derivatizations

    References 13.2

    13.3 Derivatives formation through acylation reactions

    General comments

    Some aspects regarding acylation mechanism

    Typical acylation reagents

    Derivatization with chloroformates

    Derivatization with sulfonyl derivatives

    Derivatization with isocyanates, isothiocyanates, carbonyl azides

    Artifact formation in acylation reactions

    References 13.3

    13.4 Reactions of addition to carbon-heteroatom multiple bonds involved in derivatization

    General comments

    Some aspects regarding the reaction mechanism for addition to a hetero multiple bond

    Reactions at the carbonyl group in aldehydes and ketones

    Reactions at N=C group in isocyanates and isothiocyanates

    Other reactions involving addition to a hetero multiple bond

    References 13.4

    13.5 Derivatization reactions with formation of cyclic compounds

    General comments

    Formation of nonaromatic cycles containing oxygen atoms

    Formation of aromatic cycles containing one nitrogen atom

    Reactions with the formation of azoles and related compounds

    Reactions with formation of azines and related compounds

    Reactions with formation of cyclic siliconides, cyclic phosphonothioates, and cyclic boronates

    References 13.5

    13.6 Other derivatization reactions

    General comments

    Reaction of addition to a double bond

    Oxidations and reductions


    Substitution reactions at the aromatic ring

    Complexation and formation of coordinative compounds with metal ions

    Other reactions

    References 13.6

    13.7 Derivatization reactions on solid support or involving solid phase reagents

    Derivatization on a solid phase

    Solid phase reagents

    References 13.7

    CHAPTER 14. Chemical degradation of polymers for chromatographic analysis

    14.1 Chemical degradation of polymeric carbohydrates

    General comments

    Polysaccharide structure

    Steps in polysaccharide analysis

    Identification of the constituent monosaccharides, their D or L configuration, and polymerization degree

    Determination of the position of glycosidic linkages

    Determination of the sequence of monosaccharide residues

    References 14.1

    14.2 Chemical degradation of proteins for chromatographic analysis

    General comments

    References 14.2

    14.3 Chemical degradation of other macromolecular compounds for chromatographic analysis

    General comments Degradation of nucleic acids

    Degradation of lignin

    References 14.3

    CHAPTER 15. Comments on sample preparation in chromatography for different types of materials

    15.1 Sample preparation techniques for the environmental analysis

    (air, water and soil)

    General aspects Analysis of gaseous samples

    Basic operations in sample preparation for water analysis

    Extraction of volatile and non-volatile compounds from soil samples

    Sample preparation for the analysis of various environmental pollutants

    References 15.1

    15.2 Sample preparation for the analysis of pharmaceuticals

    General aspects

    Quality control of pharmaceuticals

    Clinical trials

    References 15.2

    15.3 Sample preparation for the analysis of biological samples

    General aspects

    Handling, preservation and storage of biological samples

    Analysis of breath condensate and volatiles emitted from skin or bodily fluids

    Analysis of liquid samples of biological origin

    Analysis of solid samples of biological origins

    References 15.3

    15.4 Sample preparation for food and agricultural products

    General aspects

    Food and beverage analysis

    Agricultural products

    References 15.4

    15.5 Sample preparation related to the analysis of other materials and/or processes

    General comments

    Archeological artifacts



    Dyes and pigments


    Tobacco and cigarette smoke

    References 15.5

Product details

  • No. of pages: 696
  • Language: English
  • Copyright: © Elsevier 2021
  • Published: February 24, 2021
  • Imprint: Elsevier
  • Paperback ISBN: 9780128214053
  • eBook ISBN: 9780323898201

About the Authors

Serban Moldoveanu

Serban Moldoveanu
Dr. Serban C. Moldoveanu is Senior Principal Scientist at R. J. Reynolds Tobacco Company. His research activity is focused on various aspects of chromatography including method development for the analysis by GC/MS, HPLC, and LC/MS/MS of natural products and cigarette smoke. He has also performed research on pyrolysis of a variety of polymers and small molecules. He has over 100 publications in peer reviewed journals, eleven books, and several chapter contributions. He is a member of the editorial board of the Journal of Analytical Methods in Chemistry.

Affiliations and Expertise

Senior Principal Scientist, RJ Reynolds Tobacco Co., Winston-Salem, NC, USA

Victor David

Victor David
Dr. Victor David is a Professor and Head of the Department of Analytical Chemistry, University of Bucharest, Romania. He is the author of more than 120 publications, including 92 scientific papers in ISI international journals and 10 books and chapters in various Encyclopedias. He is also a reviewer at several international journals.

Affiliations and Expertise

Professor and Head of the Department of Analytical Chemistry, University of Bucharest, Romania

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