Supercritical fluid extraction of lipids from linseed with on-line evaporative light scattering detection

Supercritical fluid extraction (SFE) is a green alternative method of extraction for neutral lipids in seeds compared to conventional methods utilizing organic solvents. In this work, a novel method where SFE is hyphenated with an evaporative light scattering detector is presented. The method was subsequently applied to determine lipid content in crushed linseed. The new method enables rapid quantification of extracted lipids as well as be ability to continuously monitor the extraction rate in real-time, thus being able to determine the time point of completed extraction. Both the detector and the method was validated. The results show that any of several tested oils can be used to calibrate the detection method for the determination of lipids extraction from linseed. The overall method repeatability and intermediate precision was 2.6% relative standard deviations. The extracted amount was significantly less than that obtained using the standard method of Soxhlet with petroleum ether, 26.0 +/- 0.4% (95% CI, n = 9) compared to 32.3 +/- 1.3% (95% CI, n = 3) of extracted amounts. It was found that channeling effects were present, and by either performing sequential repeated extractions with decompression in-between or by using a relatively large vessel a more complete extraction could be obtained. Interestingly, a substantially higher extracted amount (approximately 50%) was obtained compared to both a single extraction by SFE and the Soxhlet method. Therefore, it is recommended that an additional extraction including a rapid decompression in-between should be included in the validation of a method using supercritical fluid extraction, in order to either rule out channeling effects or to acquire a full recovery. (C) 2014 Elsevier B.V. All rights reserved.