Automated Detection of Acrylamide in Water

Significance of the topic

Acrylamide, a known carcinogenic compound, may contaminate drinking and river water through residual monomers in polyacrylamide flocculants used in water treatment and paper manufacturing. Regulatory bodies worldwide, including the German and Austrian drinking water ordinances and the US EPA, stipulate a maximum limit of 0.1 µg/L for acrylamide. Routine, sensitive, and reproducible analysis is critical to ensure public safety and compliance.

Objectives and overview

The application note describes the development and validation of an automated solid phase extraction (SPE) workflow coupled to LC–MS/MS for acrylamide quantitation in water. Key aims include:

• Transferring a manual SPE protocol to a fully automated robotic platform (LCTech FREESTYLE SPE).
• Comparing recovery and precision metrics between manual and automated methods.
• Demonstrating compliance with DIN 38413-6 and other drinking water regulations.

Methodology and instrumentation

Sample preparation employs SPE on CHROMABOND® Carbon A cartridges. Manual conditioning, loading, and elution steps are replicated on the FREESTYLE system, which offers controlled pressure up to 4 bar to handle particulate samples. Eluates are evaporated under nitrogen at 40 °C, reconstituted in water, and analyzed by LC–MS/MS.

Chromatographic separation uses a NUCLEODUR® C18 Gravity column (150 × 3 mm, 3 µm) with a gradient from 10% to 100% methanol (0.001% formic acid) over 10 minutes. Detection is by positive-mode electrospray tandem MS (AB Sciex API 3200) in MRM mode.

Used instrumentation

• LCTech FREESTYLE BASIC with SPE module and consumables for 6 mL SPE cartridges
• Dionex Ultimate 3200 HPLC system (HPG configuration)
• AB Sciex API 3200 mass spectrometer (ESI, turbo spray)
• CHROMABOND® Carbon A cartridges and NUCLEODUR® C18 Gravity column

Main results and discussion

The automated SPE workflow achieved an average recovery of 87% for acrylamide (n = 6) with a relative standard deviation of 4%. The resulting chromatograms show a well-defined acrylamide peak with no significant interferences. Automation enabled 24/7 unattended processing, yielding high throughput and consistent performance equivalent to manual extraction.

Benefits and practical applications

The automated method reduces hands-on time, minimizes operator variability, and increases sample throughput. It meets stringent regulatory requirements for drinking water monitoring and can be adapted to other trace analytes in environmental and industrial laboratories.

Future trends and potential applications

Advances may include integration of online SPE–LC–MS workflows, incorporation of further purification modules, and application of artificial intelligence for method optimization. Such developments promise lower detection limits, faster turnaround, and broader analyte coverage.

Conclusion

The fully automated FREESTYLE SPE–LC–MS/MS method provides a robust, compliant, and efficient solution for acrylamide detection in water. It combines high recovery, good precision, and the ability to operate continuously, addressing key challenges in environmental analysis.

Reference

• Validation document for DIN 38413-6: Determination of acrylamide by high-performance liquid chromatography and mass spectrometric detection (HPLC-MS/MS).