On-surface autosampling for liquid chromatography-mass spectrometry

Area of Science:

• Analytical Chemistry
• Chromatography
• Mass Spectrometry

Background:

• Traditional chromatography methods can be time-consuming and labor-intensive.
• Integrating different chromatographic techniques offers potential for improved separation and detection.
• Advancements in open-source technology and 3D printing enable novel analytical instrumentation.

Purpose of the Study:

• To develop and validate an on-surface multi-purpose autosampler for hyphenated chromatography.
• To enable orthogonal hyphenation of normal phase thin-layer chromatography (TLC) with reversed phase high-performance liquid chromatography (HPLC) and high-resolution mass spectrometry (HRMS).
• To demonstrate the system's utility for automated analysis of complex samples.

Main Methods:

• Construction of an autosampler based on the autoTLC-MS interface, utilizing open-source hardware/software and 3D printing.
• Orthogonal hyphenation of normal phase TLC with reversed phase HPLC and HRMS.
• Application of a multi-class antibiotic mixture for calibration and detection using a Bacillus subtilis bioassay and subsequent automated elution for HRMS analysis.

Main Results:

• The autoTLC-LC-MS system successfully performed automated sequential elution of antibiotic zones.
• Intra-day precisions ranged from 2.1-14.1% and inter-day precisions ranged from 2.5-16.1% for antibiotic elution.
• The system demonstrated high sample throughput, efficiency, and reproducibility through automated operation.

Conclusions:

• The developed on-surface autosampler provides a versatile and automated solution for TLC-LC-MS hyphenation.
• This approach offers potential for planar sample clean-up, concentration, increased peak capacity, and peak purity assessment.
• The system is adaptable for analyzing leachables from various planar materials and ingredients from planar biological samples.