Screening and Individual Quantitative Works of Regulated Substances in Food Using Triple Quadrupole Mass Spectrometer LCMS-8030

Significance of the Topic

The need to screen and quantify regulated substances in food matrices such as green tea is critical for consumer safety and compliance with global regulatory standards. Advanced analytical techniques are required to detect multiple pesticides at low part-per-billion levels within complex matrices.

Objectives and Study Overview

This technical report demonstrates the application of the Shimadzu LCMS-8030 triple quadrupole mass spectrometer for screening and individual quantitation of 176 regulated agrochemicals in a green tea matrix. Ten representative pesticides were spiked at 10 and 100 ppb to evaluate detection capabilities using ultra-fast multiple reaction monitoring and generic peak detection algorithms without reliance on retention time data.

Methodology and Instrumentation

Multiple Reaction Monitoring parameters were set with a dwell time of 5 ms, pause time of 1 ms and full cycle time of approximately 2.058 seconds for 352 transitions. The HPLC separation was performed on a Shim-pack XR-ODS II column with a gradient from 30 to 95 mobile phase B over 10 minutes at 0.2 mL per minute. Ionization settings were later optimized by adjusting nebulizing and drying gas flows, temperatures and probe position to enhance sensitivity. Instrumentation details are summarized below:

• Mass Spectrometer: Shimadzu LCMS-8030 triple quadrupole
• Columns: Shim-pack XR-ODS II (75 × 2.0 mm, 2.2 µm), Shim-pack FC-ODS (150 × 2.0 mm, 3 µm)
• Mobile Phases: 5 mmol/L ammonium acetate in water and in methanol
• Flow Rate: 0.2 mL/min; Column Oven: 40 °C; Injection Volume: 1–2 µL
• MRM Transitions: 2 per compound, total 352 transitions monitored from 0 to 20 minutes

Main Results and Discussion

At 100 ppb spiking level, all ten pesticides were automatically detected using generic peak integration parameters without retention time data. At 10 ppb and a 5 ms dwell time, seven compounds were identified automatically, while three (Chlorfluazuron, Indanofan, Lufenuron) required a longer dwell time (20 ms) for reliable automatic identification. Optimization of ionization parameters resulted in approximately twofold signal enhancement and improved precision by reducing matrix interferences from caffeine. The findings underscore the balance between cycle time, dwell time and sensitivity in multiplexed pesticide screening.

Benefits and Practical Applications

The presented workflow allows simultaneous screening and quantitation of up to 100 pesticide residues per run in complex food matrices, using ultra-fast polarity switching and generic peak detection without predefined retention windows. This approach streamlines method development, reduces reliance on retention time libraries, and supports high-throughput food safety monitoring in QA/QC and regulatory laboratories.

Future Trends and Possibilities

• Integration of automated data processing algorithms with retention time prediction models to enhance identification confidence.
• Advancements in quadrupole switching speeds and shortened chromatographic methods for even greater multiplexing capacity.
• Application of high-resolution accurate mass screening to expand target lists beyond 176 compounds.
• Use of machine learning for adaptive optimization of dwell times and MRM scheduling based on sample complexity.

Conclusion

The Shimadzu LCMS-8030 system demonstrated robust performance for rapid multi-pesticide screening and quantitation in green tea, detecting all target analytes at 10 and 100 ppb levels through optimized dwell times and ionization conditions. This methodology offers a versatile platform for ensuring food safety compliance across diverse regulatory frameworks.

References

No references were provided in the original document.