Detection of Squalene and Squalane Origin with Flash Elemental Analyzer and Delta V Isotope Ratio Mass Spectrometer

Importance of the Topic

Squalane and its precursor squalene are high-value ingredients in cosmetic formulations due to their exceptional skin-hydrating properties. Reliable determination of their botanical or animal origin is critical for supporting sustainable sourcing practices and ensuring product authenticity.

Goals and Study Overview

This study aims to develop and validate a stable carbon isotope ratio (δ13C) method using elemental analysis–isotope ratio mass spectrometry (EA-IRMS) to distinguish squalene and squalane derived from shark liver oil versus olive oil. The approach also quantifies the proportion of each source in mixed samples.

Methodology and Instrumentation

• Sample preparation: approximately 200 µg of squalene or squalane weighed into tin capsules.
• Instrumentation: Thermo Scientific Flash™ 1112 EA coupled via ConFlo™ IV interface to a Delta™ V Series IRMS.
• Combustion reactor at 1020 °C with chromium oxide and silvered cobaltous/cobaltic oxide; reduction reactor at 650 °C.
• Gas separation on a 3 m Porapak QS column at 40 °C; carrier gas helium at 90 ml/min.
• Two-point calibration to the VPDB scale using IAEA-CH-6 and IAEA-CH-7 standards; analysis time ~400 s per sample.

Results and Discussion

Olive oil-derived squalene and squalane exhibited mean δ13C values of −28.06 ‰ (SD 0.06) and −27.99 ‰ (SD 0.12), respectively. Shark liver oil derivatives showed significantly higher δ13C (−20.56 ‰, SD 0.07 for squalene; −20.28 ‰, SD 0.15 for squalane). A linear correlation (R2 = 0.9993) between δ13C and the percentage of olive oil squalane enabled quantification of mixture compositions with an uncertainty of ±10 %. A 50:50 mixture produced a mean δ13C of −24.25 ‰, corresponding to 54.9 % olive oil origin.

Benefits and Practical Applications

• Authenticity testing of cosmetic raw materials
• Detection of adulteration and source blending
• Quality control in supply chain management
• Support for renewable and ethical sourcing initiatives

Future Trends and Potential Applications

Future developments may integrate high-resolution chromatographic separation for minor components, extend isotope fingerprinting to other natural ingredients, and link isotopic data to digital traceability platforms for full supply chain transparency.

Conclusion

The described EA-IRMS approach provides a precise, reliable, and rapid means to determine the origin and purity of squalene and squalane in cosmetic products, addressing both ecological and regulatory demands.

References

1. P. Jame, H. Casabianca, M. Batteau, P. Goetinck, V. Salomon, 2010. Differentiation of the Origin of Squalene and Squalane using Stable Isotopes Ratio Analysis. SOFW Journal, vol 136 1/2-2010, pp. 2-7.