FULLY AUTOMATED LIQUID-LIQUID EXTRACTION OF LOW LEVEL TRICHLORANISOLE USING GERSTEL ROBOTIC

Importance of the Topic

Trichloroanisole (TCA) is a key contributor to musty off-flavors in wine, arising from chlorinated phenolic fungicides used in cork treatment and subsequent microbial methylation. Detecting TCA at low parts-per-trillion levels is critical for environmental and food laboratories to ensure product quality and consumer safety.

Objectives and Overview of the Study

This study demonstrates a fully automated liquid–liquid extraction (LLE) workflow for trace-level TCA analysis. The goals are to reduce manual labor and improve throughput while maintaining high sensitivity and selectivity suitable for environmental and water analysis applications.

Methodology

A six-milliliter sample is transferred into a 10 mL high-recovery vial. A calibration standard is added by robotic syringe, followed by 200 µL of extraction solvent. The mixture is agitated in a QuickMix shaker for three minutes, centrifuged for five minutes, and a 10 µL aliquot of the upper organic layer is injected into the cooled injection system (PTV inlet) for GC–MS/MS analysis.

Instrumentation Used

• Gerstel Robotic Pro Dual Head autosampler
• Gerstel Cooled Injection System (CIS 4) with Programmable Temperature Vaporization (PTV)
• Gerstel QuickMix shaker
• Maestro control software
• Agilent 7890B gas chromatograph
• Agilent 7010 triple quadrupole mass spectrometer with high-efficiency source
• Anatune CF-200 centrifuge
• Agilent MassHunter Workstation software version B.07.04

Main Results and Discussion

Using the MRM transition m/z 195 → 167, the automated workflow achieved clear identification of TCA at 1 ng/L. The triple quadrupole detector provided excellent selectivity, leveraging unique chlorine isotopic patterns to minimize background interference. The measured peak-to-peak signal-to-noise ratio at 1 ng/L was 881, demonstrating robust sensitivity.

Benefits and Practical Applications

• Automation reduces hands-on time and potential for human error, increasing laboratory efficiency.
• Small sample volumes and solvent use align with green chemistry principles and cost savings.
• High sensitivity and selectivity meet stringent detection limits for environmental and food safety testing.

Future Trends and Applications

Advancements in sample automation and integration with advanced mass spectrometry platforms will further enhance throughput and analytical performance. Expanding automated LLE protocols to other trace contaminants in complex matrices can broaden the technique’s applicability in environmental monitoring and quality control sectors.

Conclusion

The fully automated LLE procedure using Gerstel robotic platforms and Agilent GC–MS/MS delivers high sensitivity and selectivity for trace TCA analysis. Automation streamlines sample preparation without sacrificing analytical performance, enabling laboratories to meet demanding regulatory and customer requirements.

Reference

Jonathan Dunscombe. Fully automated liquid–liquid extraction of low level trichloroanisole using Gerstel robotic MPS. Anatune Ltd., 2017.