Quantitation of Policosanols and Phytosterols in Brans by GC/MS

Significance of the Topic

Bran, wheat and other functional food ingredients are rich in bioactive lipids such as policosanols and phytosterols that can contribute to human health. Reliable quantitation of these compounds is essential for quality control, nutritional labelling and research into disease prevention.

Objectives and Study Overview

This work aimed to quantify six policosanols and three phytosterols in 48 bran samples using gas chromatography–mass spectrometry (GC-MS) with automated positive confirmation and to evaluate multivariate clustering to distinguish sample origins.

Used Instrumentation

• Gas chromatograph–mass spectrometer: GCMS-QP 2020 NX
• Auto injector: AOC-20i Plus
• Auto sampler: AOC-20s Plus
• Analytical column: SH-Rxi-5Sil MS (15 m × 0.25 mm i.d., 0.25 µm)
• Guard column: Rxi guard column (5 m × 0.25 mm i.d.)
• Glass insert: Topaz 3.5 mm i.d. single‐taper inlet liner with wool

Methodology and Analytical Conditions

Samples were extracted and derivatized to trimethylsilyl (TMS) ethers. GC conditions: inlet at 270 °C, splitless high pressure injection (200 kPa, 1.1 min), helium carrier (constant linear velocity 77.3 cm/s), oven ramp from 200 °C to 320 °C in 8.67 min. Injection volume 2 µL. MS operated in simultaneous scan (m/z 35–600) and selected ion monitoring (SIM) modes with ion source at 230 °C and interface at 270 °C. Automated confirmation used relative ion abundance criteria per EU 2002/657/EC.

Main Results and Discussion

Calibration curves for campesterol-TMS were linear over 0.01–10 µg/g (R² ≥ 0.9996). Flexible ion ratio settings reduced false positives and cut data‐review time by hours. Spike recoveries at 0.2 µg/g ranged from 81 % to 107 % (RSD < 14 %). Simultaneous scan data subjected to multivariate analysis (Orange) revealed four distinct sample clusters, highlighting additional marker compounds beyond the target analytes.

Benefits and Practical Applications

• Avoidance of dilution re-runs via extended dynamic range
• Automated positive confirmation expedites data review
• Robust performance in complex bran matrices
• Supports functional food development and regulatory compliance

Future Trends and Opportunities

Integration with Smart Metabolites Database™ will allow rapid addition of new analytes and automatic adjustment of retention times. Expansion of MRM/SIM workflows and application of advanced data mining and AI tools will further streamline multi-component quantitation in food, environmental and clinical matrices.

Conclusion

The GCMS-QP2020 NX platform, combined with LabSolutions Insight™, delivers accurate, high-throughput quantitation of policosanols and phytosterols in bran. Flexible ion ratio settings and extended calibration range optimize workflow efficiency and ensure reliable results for functional food research.

References

No external references cited.