Analysis of the Yerba Mate Volatile Composition Using Solid Phase Microextraction Comprehensive 2D GC–quadMS

Significance of the Topic

The volatile fraction of yerba mate contributes to its sensory profile and may harbor contaminants that pose health risks. Advanced analytical methods are essential to achieve reliable qualitative and quantitative characterization of these compounds in complex food matrices.

Objectives and Study Overview

This study aimed to develop and validate a head‐space solid‐phase microextraction (HS‐SPME) coupled with comprehensive two‐dimensional gas chromatography and quadrupole mass spectrometry (GC×GC–quadMS) method for detailed profiling of yerba mate volatiles and potential adulterants.

Methodology

The workflow included pre‐incubation of 150 mg of dry yerba mate at 80 °C for 15 min, followed by automated HS‐SPME extraction for 60 min using a DVB/CAR/PDMS fiber. Thermal desorption was performed at 250 °C in splitless mode. Chromatographic separation used two orthogonal columns with a +5 °C offset in the second oven and 6 s modulation. The quadMS detector operated in full‐scan mode (m/z 40–360) at 25 Hz.

Used Instrumentation

• Shimadzu GC‐2010 gas chromatograph × 2
• Shimadzu GCMS‐QP2010 Ultra quadrupole mass spectrometer
• Shimadzu AOC‐5000 autosampler
• Loop‐type cryogenic modulator
• SPME fiber DVB/CAR/PDMS (50/30 μm)
• Software: GCMSsolution 2.71, ChromSquare 2.0

Main Results and Discussion

The optimized method resolved over 1000 chromatographic features and tentatively identified 241 compounds using similarity and linear retention index filters. High spectral acquisition rates provided sufficient data points per peak and minimal peak skewing. A prominent band of hydrocarbon isomers and multiple polycyclic aromatic hydrocarbons indicated mineral oil contamination, likely arising during processing or drying.

Benefits and Practical Applications of the Method

• Enhanced separation and peak capacity compared to 1D GC–MS
• Rapid screening of complex matrices for flavor and contaminant profiling
• Applicable to quality control and safety assessment in food and herbal products

Future Trends and Possibilities for Use

Further developments may include integration of high‐resolution mass analyzers, automated data processing for non‐target screening, expansion to other botanicals, and advanced risk assessment studies linking chemical fingerprints to product safety.

Conclusion

The HS‐SPME GC×GC–quadMS approach offers a powerful platform for in‐depth volatile profiling of yerba mate, combining high peak capacity, reliable identification, and contaminant detection. This methodology supports comprehensive quality and safety evaluations of herbal products.

References

1. Heck J, et al. J Food Sci. 72 (2007) R138–R150.
2. Purcaro G, et al. J Sep Sci. 32 (2009) 3755–3763.