Online SPE Multi-Cartridge Kit for Fast and Easy Method Development

Importance of the Topic

This overview highlights the need for efficient sample preparation in trace-level analysis of drinking water contaminants. Conventional off-line SPE is time intensive and prone to variability, whereas integrating SPE into the LC workflow reduces manual handling, minimizes matrix effects, and extends column lifetime, essential for high-throughput analytical laboratories.

Objectives and Study Overview

This study evaluated a multi-cartridge online SPE kit designed for the Agilent 1200 Infinity Series to rapidly screen six distinct sorbent materials for the enrichment of five estrogenic compounds. Performance metrics were benchmarked against direct injection to identify the most suitable trapping column under identical chromatographic conditions.

Methodology

Water samples were spiked with five estrogens at two concentration levels and subjected to either direct injection or online SPE. The SPE platform utilized a 1290 Infinity Flexible Cube with left and right two-position valves and an external six-position cartridge selector. Chromatography employed a phenyl hexyl analytical column, and the LC/MS analysis was performed in MRM mode with optimized voltages and collision energies for each analyte.

Used Instrumentation

• Agilent 1260 Infinity Binary Pump and Standard Autosampler
• Agilent 1290 Infinity Flexible Cube with solvent selection and flush pumps
• Agilent Online SPE Multi-Cartridge Kit (6-position/14-port valve head)
• Agilent 6460 Triple Quadrupole LC/MS System with Jet Stream ionization
• Agilent MassHunter qualitative, quantitative, and optimizer software

Main Results and Discussion

Chromatographic screening revealed that PLRP-S exhibited peak tailing and Bonus RP produced low signal intensity. In contrast, C18, C8, phenyl-hexyl, and C3 phases delivered sharp peaks. Recovery for the C18 cartridge ranged from 102 to 125 percent with area RSD below 6 percent and signal-to-noise ratios comparable to direct injection. Other sorbents showed broader variability in recovery (88 to 142 percent) and higher RSD values. These results identified the C18 phase as the optimal trapping material for estrogen analysis in water.

Practical Benefits and Applications

The multi-cartridge approach accelerates method development by eliminating manual cartridge changes and system replumbing. It offers laboratories a flexible workflow for environmental monitoring, food safety testing, and pharmaceutical quality control where rapid optimization and reliable quantitation of trace-level compounds are crucial.

Future Trends and Opportunities

Future developments may include automated sorbent selection guided by data analytics, expansion to larger compound libraries, and coupling with ultra-high-pressure LC systems for even higher throughput. Integration with high-resolution mass spectrometry and AI-driven workflows can further enhance sensitivity and applicability across diverse analytical fields.

Conclusion

The Online SPE Multi-Cartridge Kit provides an efficient solution for identifying the best trapping material, delivering consistent recoveries and robust performance for estrogen detection in water. Its seamless transition between online SPE and direct injection enhances laboratory flexibility and productivity.

References

• Vigliona L et al. Analysis of natural and synthetic estrogenic endocrine disruptors in environmental waters using online preconcentration coupled with LC-APPI-MS/MS. Talanta. 2008;76(5):1088-1096.
• Naegele E. Quantification of trace-level herbicides in drinking water by online enrichment with the Agilent 1200 Infinity Series Online-SPE Solution and Triple Quadrupole MS Detection. Agilent Technologies Application Note 5991-1738EN, 2013.
• Naegele E. Comparison of Direct Injection and Online SPE for quantification by LC/MS of trace-level herbicides in water. Agilent Technologies Application Note 5991-2140EN, 2013.
• Schuhn B. High Volume Injection up to 5 mL with the Agilent 1200 Infinity Series Online SPE Solution for Highest Sensitivity. Agilent Technologies Technical Note 5991-3173EN, 2013.
• Schuhn B. Comparison of Online SPE Analysis and Direct Injection of Trace-Level Estrogens in Drinking Water with the Agilent 6460 and 6490 Triple Quadrupole LC/MS Systems. Agilent Technologies Application Note 5991-3440EN, 2013.