Analyses of Agricultural Chemicals in Golf Courses Using LC/MS/MS

Importance of the topic

Environmental monitoring of pesticide residues in golf course drainage water is essential to prevent contamination of aquatic ecosystems. Regulatory guidelines set strict limits for individual compounds, often at sub-nanogram levels. Liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) offers the sensitivity and selectivity needed to reliably quantify diverse agrochemicals at trace concentrations.

Objectives and overview of the study

This study presents both targeted individual analyses for seven selected agricultural chemicals and a simultaneous multi-component method for 44 pesticides in golf course runoff. The primary goal is to demonstrate that the LC-MS/MS approach can meet or exceed the required sensitivity defined by the Japanese Ministry of the Environment guideline for water quality.

Methodology and instrumentation

• Sample preparation: Standard mixtures prepared from certified pesticide reference solutions. Polypropylene vials used to minimize adsorption.
• Chromatography: Reverse-phase UHPLC with Shim-pack Scepter or XR-ODS columns (100 mm × 2.0 mm, sub-2 µm) and binary gradients of ammonium acetate buffer (2–5 mmol/L) and organic solvents (methanol or acetonitrile).
• Mass spectrometry: Shimadzu LCMS-8050 triple quadrupole with electrospray ionization in positive or negative mode. Multiple reaction monitoring (MRM) transitions optimized for each analyte. Dwell times and collision energies adjusted for peak sensitivity.

Main results and discussion

• Individual methods for seven compounds achieved method detection limits between 0.0001 and 0.0025 mg/L, with reproducibility (%RSD) below 4% and calibration linearity (r²) above 0.997.
• Simultaneous analysis of 44 pesticides showed quantitation down to 0.0002 mg/L for most analytes (%RSD < 14%), covering water quality criteria at one-hundredth of guideline values.
• Typical chromatograms demonstrated clear separation and absence of significant matrix interferences, confirming method robustness.

Benefits and practical applications of the method

• High throughput: Individual and multi-analyte runs completed within 20 minutes, enabling routine monitoring.
• Regulatory compliance: Meets sensitivity requirements for environmental surveillance of golf course effluents.
• Versatility: Applicable to various agrochemicals with minimal method modification.

Future trends and potential applications

Advances in high-resolution mass spectrometry, automation of sample preparation, and data processing by machine learning will further enhance throughput and expand analyte coverage. Integration with real-time sensor networks may enable continuous monitoring of pesticide runoff.

Conclusion

The validated LC-MS/MS methods deliver precise and accurate quantitation of both targeted and broad-spectrum pesticide panels at levels well below regulatory limits. These approaches support effective water quality management in golf course environments.

Instrumentation used

• Shimadzu UHPLC Nexera X2
• Shimadzu LCMS-8050 triple quadrupole mass spectrometer
• Shim-pack Scepter C18-120 and Shim-pack XR-ODS columns

References

1. Ministry of the Environment, Japan. Guideline for the Prevention of Water Pollution and Damage to Aquatic Animals and Plants by Agricultural Chemicals Used in Golf Courses, Soil Environment Management Division, Environment Management Bureau, MOE, Final amendment Nov. 30, 2018.
2. Ministry of the Environment, Japan. Water quality standards for agricultural chemicals, accessed April 18, 2019.
3. Ministry of the Environment, Japan. Standard Analysis Methods for Drainage Water, Addendum to Guideline No. 1811301, accessed April 18, 2019.