Modern Sample Preparation for Chromatography
- 2nd Edition - March 1, 2021
- Latest edition
- Authors: Serban C. Moldoveanu, Victor David
- Language: English
- Paperback ISBN:9 7 8 - 0 - 1 2 - 8 2 1 4 0 5 - 3
- eBook ISBN:9 7 8 - 0 - 3 2 3 - 8 9 8 2 0 - 1
Modern Sample Preparation for Chromatography, Second Edition explains the principles of sample preparation for chromatographic analysis. A variety of procedures are applied to mak… Read more
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.
- 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 sectorsPost graduate and upper undergraduate students in analytical chemistry
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 commentsSampling 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
Weighing
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
Injectors
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
Sieving
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
Distillation under vacuum plus centrifugal force
Steam distillation and other distillation processes
Vaporization
Drying and freeze-drying
Cryofocusing
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
Composites
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
Adsorbents
Other types of conventional sorbents used for SPE
Monolithic materials
Electrospun nanofibers
Fabrics
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
Dialysis
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
Hydrolysis
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 analysis14.1 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
Cosmetics
Detergents
Dyes and pigments
Preservatives
Tobacco and cigarette smoke
References 15.5
- Edition: 2
- Latest edition
- Published: March 1, 2021
- Language: English
SM
Serban C. Moldoveanu
Serban C. Moldoveanu was Senior Principal Scientist at R. J. Reynolds Tobacco Company, USA, and retired at the end of 2023. His research activity was 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 written over 150 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 and of Frontiers in Chemistry.
Affiliations and expertise
Senior Principal Scientist, RJ Reynolds Tobacco Co., Winston-Salem, NC, USAVD
Victor David
Victor David was a Professor and Head of the Department of Analytical Chemistry, University of Bucharest, Romania. Recently retired, he remains Emeritus Professor at the same Department. His main field of research is separation science (theory and applications in various scientific domains). He is the author of more than 200 publications, including over 150 scientific papers in peer reviewed journals and 25 books and chapters. He is member of editorial board of Biomedical Chromatography, Molecules, Journal of Essential Oil-Bearing Plants and Revue Roumaine de Chimie.
Affiliations and expertise
Professor and Head of the Department of Analytical Chemistry, University of Bucharest, RomaniaRead Modern Sample Preparation for Chromatography on ScienceDirect