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Sample Preparation for HPLC and GC

Sample preparation, while essential, consumes resources – time, effort, and funds – and significantly impedes method throughput.

So the cardinal rule in the development of analytical methods for HPLC or GC is to minimize sample preparation whenever possible.

Nevertheless, in scenarios involving complex matrices, sample preparation becomes inevitable.


In such instances, ingenuity is paramount in crafting solutions that strike a delicate balance between sample quality and method cost-effectiveness.


This guide endeavors to furnish you with invaluable insights into navigating the intricate tasks of extraction, sample cleanup, and pre-concentration in real-world scenarios.


Best wishes for success,
The Author


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Table of Contents

1.1. Preliminary Sample Processing


1.2. Liquid-Liquid Extraction (LLE)


1.2.1. Basics of LLE Method
1.2.2. Application of Liquid-Liquid Extraction in Sample Preparation. Advantages and Disadvantages of Liquid-Liquid Extraction
1.2.3. Traditional LLE Techniques. Liquid-Liquid Microextraction. Liquid-phase microextraction.
1.2.4. Concentration of the sample by solvent evaporation: techniques, limitations. Solvent replacement.

1.3. Emulsion and Coagulation Structure Disruption


1.3.1. Types of Dispersed Systems
1.3.2. Techniques for Disrupting Dispersed Systems


1.4. Liquid Extraction of Solid Matrices


1.4.1. Specifics and Techniques of Liquid Extraction of Solid Matrices
1.4.2. Technical implementation of solid matrix extraction. Traditional systems. Automated pressurized extraction systems.

1.5. Extraction of Volatile Components


1.5.1. Static and Dynamic Headspace Extraction
1.5.2. Steam Distillation
1.5.3. Solid-Phase Microextraction, SPME


1.6. Adsorption Sample Preparation Methods: Adsorption Cleanup (AC) and Solid-Phase Extraction (SPE)

1.6.1. Fundamentals of SPE and AC Methods
1.6.2. SPE Procedure
1.6.3. Online SPE for HPLC
1.6.4. Adsorption Modes Retention Mechanism SPE and AC in Normal-Phase (NP) Mode SPE and AC in Reversed-Phase (RP) and Mixed RP/Exclusion Modes Charge Transfer (CT) and Anion-Exchange (AE) Modes SPE in Ionic and Mixed Ionic/Reversed-Phase Modes

1.6.5. Adsorption Materials for SPE and AE; Their Application Variants in Different Adsorption Modes Organic Polymer Adsorbents: Neutral and Bifunctional. Carbon Materials Restricted access media (RAM) adsorbents of various types
1.6.6. Development of SPE Procedure

1.7. Highly efficient chromatographic sample preparation methods

1.7.1. Low-pressure column chromatography (LC)
1.7.2. Exclusion Chromatography
1.7.3. Two-Dimensional HPLC and HPLC-GC


1.8. Ultrafiltration Sample Preparation Methods


1.9. Methods Based on Chemical Derivatization


2.1. Representation of the sample preparation algorithm as a block diagram. Two diagrams of typical approaches to sample preparation for cases of aqueous and non-aqueous matrices.

2.2. Extraction of non-polar target compounds from aqueous media using the example of determining various groups of persistent organic pollutants: PCBs, PAHs, PCDDs, PCDFs, PAHs, and HOPs in wastewater by GC/MS.

2.3. Extraction of Non-Polar Target Compounds from Polar Matrices Using the Example of Determining Pesticides of the OCP, OPP, and Triazine Groups in Plant Matrices by the QuEChERS-GC/MS/EC Method.

2.4. Extraction of polar target compounds from aqueous media using the example of patulin determination in juices by SPE-HPLC/UV.

2.5. Extraction of non-polar target compounds from non-aqueous matrices using the example of determining PAHs in fatty products and smoked preparations by SPE-HPLC/FLD and SPE-GC/MS.

2.6. Extraction of polar target compounds from non-aqueous matrices using the example of determining furfural derivatives in mineral oils by SPE-HPLC/UV

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