Shimadzu Liquid Chromatograph Mass Spectrometer LCMS-8045 - Application Booklet

Significance of the Topic

The widespread use of carbamate pesticides in agriculture poses environmental and health risks due to their persistence and toxicity. Soils act as both a sink and source of these contaminants, affecting crop safety and water quality. Rapid, sensitive methods for multi-residue analysis in soil are crucial for monitoring and controlling pesticide pollution.

Objectives and Study Overview

This work establishes a fast, reliable method to simultaneously quantify 20 carbamate pesticides in soil samples. The goal is to achieve high sensitivity, selectivity, and throughput using state-of-the-art UHPLC coupled with triple quadrupole mass spectrometry.

Methodology and Instrumentation

The analysis employs Shimadzu’s UHPLC LC-30A system with a Shim-pack XR-ODS III column (2.0×75 mm, 1.6 μm) and a Nexera XR triple quadrupole mass spectrometer (LCMS-8045). Key parameters:

• Mobile phase A: 5 mM ammonium acetate in water; B: methanol
• Gradient elution: 20 %→95 % B over 6 min, total runtime 12 min
• ESI positive mode with MRM transitions optimized for 20 analytes
• Solid-phase extraction cleanup of soil extracts

Main Results and Discussion

Calibration demonstrated excellent linearity (r² > 0.997) over 0.25–200 µg/L for all 20 compounds. Limits of detection ranged from 0.005 to 0.359 µg/L, and limits of quantitation from 0.012 to 1.086 µg/L. Precision tests (n = 6) yielded retention time RSDs of 0.015–0.263 % and peak area RSDs of 0.554–5 %. Matrix spike recoveries in soil (2 µg/kg and 16 µg/kg) were within 88.1–108.4 %, confirming method accuracy.

Benefits and Practical Applications

This approach enables rapid, high-throughput monitoring of carbamate residues in soils, supporting regulatory compliance and environmental risk assessments. Its sensitivity and robustness make it suitable for routine surveillance and remediation studies.

Future Trends and Potential Uses

Expanding the pesticide panel to include emerging and legacy compounds will further enhance environmental monitoring. Combining this method with automation and high-resolution mass spectrometry could enable non-targeted screening for comprehensive soil contaminant profiling.

Conclusion

The described UHPLC-MS/MS method achieves sensitive, accurate, and high-speed analysis of 20 carbamate pesticides in soil. Its excellent linearity, precision, and recovery meet stringent regulatory standards, providing an effective tool for environmental monitoring and risk assessment.