Application Notebook - Solutions for Food Development

Importance of the Topic

Food product development and quality assurance depend heavily on reliable, high‐throughput analytical methods. Techniques such as high‐performance liquid chromatography (HPLC), gas chromatography (GC), and liquid chromatography–mass spectrometry (LC–MS) provide sensitive, selective, and simultaneous analysis of vitamins, sugars, sweeteners, lipids, amino acids, biogenic amines, flavor compounds, and contaminants in complex food and beverage matrices.

Study Overview and Aims

This application notebook collects multiple case studies demonstrating advanced chromatographic and mass spectrometric solutions for food analysis. Key objectives include:

• Developing HPLC methods for simultaneous water‐soluble vitamin analysis without ion‐pair reagents
• Profiling mono‐ and oligosaccharides in juices, energy drinks, sake, and dietary fiber formulations
• Quantifying low‐molecular‐weight soluble dietary fiber and multiple artificial sweeteners by LC–MS/MS
• Analyzing biogenic amines (histamine, tyramine) via post‐column fluorescence derivatization
• Profiling aroma volatiles in sake by headspace GC‐FID and GC‐MS
• Comparing GC columns for alcoholic beverage congener profiling
• Introducing Nexis GC‐2030, a high‐sensitivity, high‐throughput GC platform
• Applying two‐dimensional LC (Nexera‐e) for polyphenol, lipid, and carotenoid separations
• Establishing rapid chiral amino acid separations by column switching
• Implementing metabolomic workflows for primary and secondary food metabolites
• Multicomponent profiling of beer metabolites and spectroscopic fingerprinting of olive oils

Methods and Instrumentation

The studies employed a range of instruments and techniques:

• Reversed‐phase HPLC with novel columns (Shim‐pack MAqC‐ODS I, XR‐ODS Ⅱ)
• Ligand‐exchange sugar analysis columns (Shim‐pack SCR‐101N, SPR‐Ca, SPR‐Pb)
• Differential refractive‐index (RID), evaporative light‐scattering (ELSD), and UV‐VIS detection
• Triple‐quadrupole LC–MS/MS (LCMS‐8040, LCMS‐8050, LCMS‐8060) for sweeteners, amino acids, metabolites
• Highly sensitive GC‐FID and GC‐MS (Prominence‐i, GC‐2030, GCMS‐TQ8040, Nexera GC×GC) for volatiles, congeners, oligosaccharides
• Comprehensive 2D‐LC (Nexera‐e) for peak purity and complex mixture resolution
• Chiral amino acid analysis with column switching valves (CROWNPAK CR‐I +/−)
• Headspace sampling and post‐column derivatization (OPA, diacetyl reagent DS‐DA)
• Spectroscopic profiling using UV‐VIS and spectrofluorophotometry

Main Results and Discussion

Key findings across the case studies include:

• Simultaneous separation of eight water‐soluble vitamins in 15 min without ion‐pair reagents
• Quantitative sugar profiling in fruit juices and beverages with high linearity using RID
• Energy drink analysis for sugars and polyols using SPR‐Pc columns and RID
• Oligosaccharide profiling in Japanese sake by ELSD and quantitation to low mg/L levels
• Rapid HPLC analysis of low‐molecular‐weight soluble dietary fibers in beverages
• Simultaneous quantitation of 9 and 16 artificial sweeteners by LC–MS/MS with LLOQs at sub‐ng/mL
• Sensitive analysis of histamine and tyramine in sauces, wines, and soy products via post‐column fluorescence
• Headspace GC‐FID aroma profiling of sake distinguishing key volatile markers
• Alcohol congener comparison across beverages using multiple GC columns
• High‐sensitivity FID and streamlined GC workflows on Nexis GC‐2030
• Comprehensive 2D‐LC separation of polyphenols in red wine, triglycerides in oils, and carotenoids in chili
• Chiral D/L amino acid separations in fermented foods using column switching with full automation
• Automated UHPLC–MS/MS workflows for simultaneous primary and secondary metabolite profiling in citrus
• Metabolomic tracking of sulfur‐containing pathways in engineered E. coli cultures
• Multivariate classification of beer metabolite profiles and spectroscopic differentiation of olive oils

Benefits and Practical Applications

The methods provide food and beverage researchers and QA/QC laboratories with:

• High‐throughput, robust platforms for multicomponent analysis
• Enhanced sensitivity and reproducibility for trace‐level compounds
• Reduced sample prep via online or automated headspace, derivatization, and column switching
• Comprehensive 2D‐LC solutions for resolving coeluted analytes in complex matrices
• Real‐time data analysis and multivariate screening for rapid food authenticity and quality evaluation

Future Trends and Potential Uses

Emerging directions include:

• Integration of LC–MS‐based metabolomics with AI‐driven data analysis for predictive food quality models
• Miniaturized and inline sample preparation for on‐site testing and real‐time process monitoring
• Expansion of 2D chromatographic techniques to new food bioactives and contaminants
• Advances in high‐resolution MS for non‐targeted profiling and unknown compound identification
• High‐throughput automation of chiral and derivatized analyses for enantiomeric purity in nutraceuticals

Conclusion

Shimadzu’s comprehensive toolkit of chromatographic and spectroscopic analytical solutions demonstrates the ability to address a wide range of food and beverage quality challenges. By providing sensitive, selective, and high‐throughput methods for simultaneous multi‐component analysis, these technologies support regulatory compliance, product development, and food authenticity testing, while paving the way for future advances in metabolomics and data‐driven food science.