Using Peak Deconvolution of Photodiode Array Data to Attain Faster, Easier Performance of EPA Method 8330B

Importance of the Topic

Effective detection of low-level explosive residues in environmental matrices is essential for public health protection and contamination control.

Objectives and Study Overview

This application demonstrates accelerated EPA Method 8330B analysis by incorporating peak deconvolution of photodiode array data, aiming to reduce development time and improve quantitation of coeluting nitroaromatics, nitramines, and nitrate esters.

Methodology and Instrumentation

A Shimadzu Nexera-I MT 3D HPLC system with an LC-2040 PDA detector served as the platform. A primary C-18 column (2.1×200 mm, 5 μm) with a methanol/water mobile phase, including low percentages of acetonitrile, was optimized at 42 °C. LabSolution LC software with i-PDeA II performed multivariate curve resolution alternating least squares deconvolution.

• Column: C-18 (ODS)
• Detection: PDA at 254 nm (most analytes) and 210 nm (nitrate esters)
• Software: LabSolution LC with i-PDeA II module

Main Results and Discussion

Baseline separations were incomplete, with overlapping peaks for compounds such as Tetryl, NG, TNT isomers, and dinitrotoluenes. Deconvolution resolved these overlaps effectively, achieving spectral similarity indices above 0.999 and calibration linearity (R2 ≥ 0.999) over 2–500 ng on column (2–250 ng for amino isomers).

Benefits and Practical Applications

Peak deconvolution eliminates the need for multiple confirmation columns and extensive method adjustments. It ensures accurate quantitation and spectral verification even for poorly resolved analytes, streamlining QA/QC workflows in environmental analysis.

Future Trends and Possibilities

Combining chemometric deconvolution with UHPLC or high-resolution mass spectrometry may further accelerate analyses and lower detection limits. Automated data processing will support field-deployable screening for rapid environmental monitoring.

Conclusion

Implementing PDA-based deconvolution in EPA Method 8330B significantly reduces method development time while providing reliable quantitation and spectral confirmation of explosive residues.

Reference

Shimadzu Application Note No. HPLC-023 High Performance Liquid Chromatography Using Peak Deconvolution of Photodiode Array Data to Attain Faster, Easier Performance of EPA Method 8330B April 2019