New Developments in GC, HPLC and Sample Prep at Supelco

Significance of Topic

Modern analytical laboratories rely on robust separation techniques to deliver accurate qualitative and quantitative results in diverse fields such as environmental monitoring, food safety, pharmaceuticals and industrial quality control. Advances in gas chromatography (GC), liquid chromatography (HPLC) and sample preparation strategies directly impact analytical efficiency, sensitivity and throughput. Ionic liquid stationary phases offer novel selectivity patterns in GC, while next-generation HPLC particles and specialized sample prep workflows reduce matrix effects and extend column lifetime. Reliable air sampling methods for reactive analytes complete the analytical chain. The integration of these developments supports regulatory compliance and high-throughput screening in research and production.

Study Objectives and Overview

This presentation reviews recent Sigma-Aldrich developments across five key areas:

• Design and performance of ionic liquid capillary columns for GC applications
• Innovations in solid-phase microextraction (SPME) fiber technologies
• Introduction of Titan™ UHPLC columns with narrow particle size distribution
• Advances in solid-phase extraction (SPE) including HybridSPE-PL and enhanced QuEChERS sorbents
• Deployment of the ASSET™ EZ4-NCO dry sampler for isocyanate monitoring

The goal is to highlight how these tools improve method selectivity, reproducibility, and workflow efficiency.

Methodology and Used Instrumentation

• Ionic liquid GC columns (SLB-IL60, SLB-IL111, SLB-IL59, SLB-IL94, SLB-IL107, SLB-IL200) evaluated by capillary GC with FID or TCD detection; carrier gases hydrogen or helium
• Comparative studies of cis/trans fatty acid methyl esters (FAMEs), polycyclic aromatic hydrocarbons (PAHs) and volatile organics
• GC×GC/TOFMS analyses using a LECO Pegasus system for two-dimensional separations of biodiesel constituents
• SPME fiber development including sol-gel and HPLC particle coatings; automated DESI-1D source coupling
• HPLC and UHPLC performance tests on Dionex 3000 systems using Titan C18 columns (1.9 µm porous silica, fused-core 2.7 µm, 5 µm particles)
• HybridSPE-PL plates and cartridges with zirconia-coated silica for phospholipid removal; QuEChERS cleanup sorbents (PSA, C18, Z-Sep, Z-Sep+, Z-Sep/C18 mixtures)
• ASSET EZ4-NCO dry sampler for derivatization of isocyanates with dibutylamine; analysis by LC-MS

Main Results and Discussion

• Ionic liquid columns demonstrated complementary separation patterns compared to conventional phases, with enhanced resolution of cis/trans FAME isomers, PAH isomers and water-soluble volatiles under isothermal and temperature-programmed conditions
• SLB-IL60 and SLB-IL111 exhibited unique selectivity for unsaturated lipids and aromatic compounds, enabling shorter analysis times for complex matrices
• GC×GC/TOFMS with non-polar/polar or polar/non-polar column sets achieved detailed profiling of biodiesel components including saturates, aromatics and esters
• SPME fibers with biocompatible binders resisted swelling and allowed single-use in vivo sampling; pipette tip formats and holders for automated DESI coupling streamlined extraction for HPLC or MS detection
• Titan porous silica particles produced by the Ecoporous™ process achieved narrow particle size distribution (D90/D10 < 1.15) without post-sizing; Titan C18 columns delivered higher efficiency and lower backpressure compared to 1.7 µm competitors in MeOH and ACN
• HybridSPE-PL effectively removed proteins and phospholipids, maintaining stable backpressure, reducing ion suppression and eliminating the need for post-run column cleaning; small-volume formats improved throughput
• Enhanced QuEChERS sorbents (Z-Sep, Z-Sep+, Z-Sep/C18) offered superior cleanup of fatty and pigmented food extracts, as demonstrated in avocado pesticide analysis
• The ASSET EZ4-NCO dry sampler provided complete derivatization of vapour and particulate isocyanates, enabling accurate personal monitoring of aliphatic and aromatic diisocyanates with minimal field handling

Benefits and Practical Applications

• Improved method selectivity reduces co-elution and simplifies data interpretation
• Higher chromatographic efficiency allows faster throughput and lower solvent consumption
• Robust sample preparation workflows decrease matrix effects and extend column lifetime
• Modular SPME and air sampling devices support in vivo and workplace exposure studies
• Enhanced sorbents enable reliable pesticide screening in complex food matrices
• Adoption of these technologies accelerates compliance with regulatory requirements in pharmaceutical, environmental and food laboratories

Future Trends and Possibilities

The continued evolution of stationary phases and sample prep platforms is expected to focus on:

• Tailored ionic liquid phases for specific analyte classes and two-dimensional GC applications
• Integration of automated SPME devices with ambient mass spectrometry techniques
• Design of sub-2 µm porous particles for ultra-high throughput UHPLC at moderate pressures
• Development of mixed-mode and hybrid sorbents for comprehensive extraction of polar and non-polar residues
• Portable air samplers coupled with on-site MS detection for real-time exposure assessment

Conclusion

Sigma-Aldrich’s portfolio of ionic liquid GC columns, next-generation SPME fibers, Titan porous silica UHPLC media, specialized SPE workflows and the ASSET EZ4-NCO sampler collectively enhance analytical performance and workflow efficiency across a range of applications. These innovations deliver greater separation power, reduced matrix interference and streamlined protocols, meeting the demands of modern analytical laboratories.

References

• Desmet R., et al. J Chromatogr A 1217 (2010) 7074-7081
• Little J.L., et al. J Chromatogr B 833 (2006) 219-230