Shimadzu LC World Talk 2011 Issue 1

Significance of the topic

The rapid growth in complex sample analysis demands analytical methods that deliver high sensitivity, speed and reliability. Triple quadrupole mass spectrometry has become essential for trace-level quantitation in diverse matrices, while ultra-high-performance liquid chromatography (UHPLC) pushes chromatographic speed and resolution. Combining these technologies with advanced automation and connectivity enhances productivity and supports critical applications, including pharmaceutical impurity control, in vivo monitoring of biomarkers and food safety testing.

Objectives and overview of the article

This newsletter highlights Shimadzu’s latest advances: the LCMS-8030, an ultra-fast triple quadrupole mass spectrometer; the Nexera UHPLC system; automated HPLC analysis of microdialysis samples for circadian studies; structural and quantitative analysis of genotoxic impurities in compliance with FDA guidelines; rapid melamine detection in pet food; and remote system monitoring via iPad.

Methodology and instrumentation used

— LCMS-8030 triple quadrupole MS coupled to Nexera or Prominence HPLC
— UFsweeper collision cell technology for fast MRM and polarity switching
— Nexera UHPLC delivering up to 130 MPa pressure, sub-2 µm column compatibility, rapid autosampler and column oven control
— Long-term microdialysis sampling in freely moving rats with dual‐channel peristaltic pumps, VICI 10-port sample valve and reversed‐phase HPLC with fluorescence detection
— 2D-LC/LCMS-IT-TOF for structural elucidation of ultra-trace pharmaceutical impurities, with on-line desalting and fractionation
— Co-Sense for Impurities system for automated trapping and concentration of trace impurities using dual-dimension HPLC and UV detection
— Rapid HILIC‐based LC/MS/MS method for melamine and cyanuric acid quantitation in food samples
— LabSolutions software and iPad interface for networked instrument control and maintenance scheduling

Key results and discussion

• The LCMS-8030 achieved 1 ms MRM dwell times, 15 ms polarity switching and 15,000 u/s scan speed, enabling quantitation of 226 pesticides in two minutes with high linearity (4.5 orders of magnitude) and minimal cross talk.
• UFsweeper technology maintained sensitivity at 1 ms dwell time and delivered over 500 MRM transitions per second.
• Long-term stability tests of pesticide spikes in tomato extract (1 µL injections, 1,400 cycles, 47 hours) showed <2.2% RSD.
• Nexera UHPLC demonstrated ultra-high speed (50 MPa) and ultra-high resolution (118 MPa) separations with retention time RSD <0.1% and injection volume RSD at 0.1 µL steps.
• Automated microdialysis HPLC analyzed rat pineal dialysates every 20 minutes for up to two months, generating high-resolution melatonin, serotonin and N-acetylserotonin profiles for precise circadian phase determination.
• 2D-LC/LCMS-IT-TOF successfully fractionated phosphate-buffered impurities and delivered accurate MSn and high-resolution mass data for structural identification of sulfonamide drug impurities at 0.1% levels.
• Co-Sense for Impurities offered 10–20× sensitivity enhancement for trace compounds (e.g., methyl paraben) through online trapping and dual-column concentration.
• The rapid HILIC LC/MS/MS method quantified melamine and cyanuric acid in pet food with 60 s run time, LOQ <50 ppb and recoveries >90%.
• Shimadzu’s LabSolutions network and iPad app enabled batch monitoring of up to multiple UHPLC/HPLC systems, remote cleaning and maintenance planning, improving uptime and workflow efficiency.

Benefits and practical applications of the method

• High-throughput trace analysis for environmental, food safety and pharmaceutical QA/QC
• Real-time in vivo monitoring for neuroscience and pharmacology studies
• Compliance with evolving genotoxic impurity guidelines via precise structural characterization and quantitation
• Reduced instrument downtime through simplified maintenance and remote control
• Enhanced laboratory productivity with ultra-fast separation, data acquisition and processing

Future trends and potential applications

• Further integration of multi-dimensional separations and high-resolution MS for comprehensive impurity profiling
• Advanced automation and AI-driven data analysis to accelerate method development and result interpretation
• Expansion of real-time bioanalytical monitoring platforms for clinical and preclinical research
• Deeper connectivity between instruments, lab information systems and mobile devices for remote operation and data sharing
• Continuous improvements in UHPLC column technology and MS sensitivity to drive speed and robustness

Conclusion

Shimadzu’s latest solutions combine ultrafast chromatography, high-throughput mass spectrometry, advanced automation and mobile connectivity to address modern analytical challenges. These innovations deliver unprecedented speed, sensitivity and reliability for trace quantitation, structural identification, in vivo monitoring and remote system management, paving the way for more efficient workflows across pharmaceutical, environmental, food safety and life science laboratories.

References

1. Borjigin J, Liu T (2008) Application of long-term microdialysis in circadian rhythm research. Pharmacol Biochem Behav 90:148–155.
2. Chin JR (1990) Determination of six indolic compounds, including melatonin, in rat pineal using high-performance liquid chromatography with serial fluorimetric-electrochemical detection. J Chromatogr 528:111–121.
3. Liu T, Borjigin J (2005) Reentrainment of the circadian pacemaker through three distinct stages. J Biol Rhythms 20:441–450.
4. Liu T, Borjigin J (2006) Relationship between nocturnal serotonin surge and melatonin onset in rodent pineal gland. Journal of Circadian Rhythms.