A cartridge-based device for automated analyses of solid matrices by online sample prep-capillary LC-MS/MS

Area of Science:

• Analytical Chemistry
• Environmental Science

Background:

• Sample preparation is critical but often laborious, time-consuming, and error-prone.
• Automated and miniaturized techniques offer greener alternatives, but often overlook solid samples.
• Integrating sample preparation with analysis streamlines workflows.

Purpose of the Study:

• To develop and validate an automated, miniaturized platform for solid sample preparation and analysis.
• To combine sample preparation and capillary liquid chromatography-mass spectrometry (LC-MS) into a single system.
• To extract and analyze pesticides in soil samples.

Main Methods:

• A cartridge packed with soil samples was coupled with capillary LC-MS.
• A fractional factorial design followed by a central composite design was used for method optimization.
• Nine pesticides commonly used in sugarcane crops were targeted for extraction and analysis.

Main Results:

• The optimized method achieved linear ranges from 10 to 125 ng g⁻¹ with R² > 0.985.
• Accuracy and precision met International Council for Harmonisation (ICH) Q2(R1) standards.
• The approach demonstrated effectiveness for pesticide extraction and analysis in soil.

Conclusions:

• The proposed integrated platform is effective for the automated and miniaturized preparation and analysis of pesticides in solid matrices.
• The method shows potential for application to other solid samples, such as honeybees.
• This work advances greener analytical chemistry by addressing the challenges of solid sample preparation.