Sample Prep Summer School: Introduction

Summer School: Automation and miniaturization in sample preparation
 

Summer School 2023:
Automation and miniaturization in sample preparation

Introduction

Automation of extraction procedures significantly saves times and sample handling to increase the throughput and repeatability of analyses while avoiding errors. This course will be organized in 3.5 days to cover a variety of approaches to sample preparation. In the first part lectures will be focused to SPE directly connected (on-line) to LC separations. Two different ways how to connect SPE to LC will be discussed – either column switching directly in the LC system or oof-line SPE using different sorbent materials including nanofibers. The other extraction area will be more focused on the green approach of supercritical fluid extraction (SFE) applicable to lipophilic as well as hydrophilic target analytes. Modification of the extractant with modifiers and variation of pressure and temperature – viscosity and lipophilicity will be tested in practical tasks while via lectures, the principles of SFE, instrumentation, and method development will be explained including limitations and possibilities in case of hydrophilic substances extraction that are mainly present in plant extracts (polyphenolic compounds). In case of this analyte class, SFE provides an alternative way of extraction to classical solvent-based approaches allowing the extraction also of non-stable substances with a minimum risk of decomposition.

In the second part of the course, the automation and miniaturization of liquid phase microextraction approaches by flow automation techniques will be explained in a thorough lecture and accompanied by demonstration of a Lab-In-Syringe system covering dispersive liquid-liquid microextraction and single drop microextraction including the use of green solvents for this purpose and the use of 3D printing technology for system setup and optimization. The automation of dispersive solid phase extraction by this technique will further be shown. Short seminar concerning greenness evaluation of different sample preparation approaches will conclude advantages and disadvantages in terms of practical applications of the mentioned extraction techniques for routine analysis.

The last part of the summer school will be devoted to practical tasks in frames of workshop organized in laboratories of the Department of Analytical Chemistry while the individual task will be focused to:

  1. LC-SPE – column-switching mode
  2. SPE sorbents manipulation, filled pipette tips (SPE) + MEPS
  3. Supported liquid extraction
  4. Supercritical Fluid Extraction
  5. Lab-In-Syringe-DLLME + demonstration of other LIS automated sample preparation methods
  6. Sequential Injection Analysis applied to automated SPE

Practical tasks will further cover SPE attempting miniaturization using different nanofibrous polymers such as polyethylene, polyamide, or polycaprolactone for the extraction of pesticides/insecticides or bisphenols.

Aims

The aims of this course are:

  • to extend and increase the theoretical and experimental knowledge based on green sample preparation including on-line SPE, LPME, and SFE techniques as well as on the automation and miniaturization of liquid phase microextraction approaches

  • to support confidence of participants to modern extraction methods

  • to show and highlight modern advances in sample preparation in a variety of application fields

  • to stress modern alternatives of sample preparation in frames of SPE using advanced/smart materials (e.g., nanofiber materials)

  • to demonstrate advantages of SFE in extraction of lipophilic or low stability hydrophilic analytes

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