Analysis of Clopyralid in Manure Compost and Sludge Fertilizer

Význam tématu

Monitoring clopyralid residues in manure-based amendments is essential for environmental protection, food safety and compliance with regulatory standards.

Cíle a přehled studie

This study aims to establish a robust LC-MS/MS method for trace-level determination of clopyralid in cattle, pig and horse manure composts, as well as composted sludge fertilizer.

Použitá instrumentace

• HPLC: Nexera X3 system with Shim-pack Scepter C18-120 column (100 × 2.1 mm, 1.9 µm).
• Mass spectrometer: LCMS-8050 with ESI source in positive mode, operating in MRM.

Metodika

• Mobile phases: A) 0.1 % formic acid in water; B) methanol.
• Gradient: 5 % B at 0 min → 60 % at 5 min → 95 % at 6 min → 5 % from 7 to 10 min → re-equilibration to 17.01 min.
• Flow: 0.4 mL/min; Column temperature: 40 °C; Injection: 5 µL.
• Valve switching to introduce analyte between 1.4 and 5.5 min, removing matrix outside this window.
• MRM transition: m/z 191.90 → 110.10 (CE −21 V); Interface voltage: 3.0 kV; Interface temperature: 400 °C; DL & block heater: 150 °C; Nebulizing: 3 L/min; Drying & heating: 10 L/min.

Hlavní výsledky a diskuse

The method provided clear separation and quantification of clopyralid in all tested compost and sludge matrices. Retention times between 1.4 and 5.5 min yielded reproducible signals with low background noise, demonstrating effective matrix elimination by valve switching. Performance parameters such as limits of detection, quantitation and recovery rates meet common regulatory criteria.

Přínosy a praktické využití metody

• Short analysis time (<20 min per sample) with minimal sample preparation.
• High sensitivity and selectivity for routine QA/QC in agricultural and environmental labs.
• Reduced maintenance due to selective analyte introduction.

Budoucí trendy a možnosti využití

Future developments may include automated sample pre-treatment, extension to multi-residue profiling, adoption of green solvents, and integration with advanced data analytics for automated compliance monitoring.

Závěr

The described LC-MS/MS approach using Shimadzu instrumentation delivers a reliable, efficient and high-throughput solution for monitoring clopyralid in nutrient-rich amendments, aiding environmental safety and regulatory compliance.

Reference

• Application News 01-00352, Shimadzu Corporation.