Determination of lignans in flaxseed using liquid chromatography with time-of-flight mass spectrometry

• Published in: Journal of Chromatography A Vol. 1216; no. 2; pp. 217 - 229
• Main Authors: Popova, I.E., Hall, C., Kubátová, A.
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 09.01.2009; Amsterdam; New York: Elsevier; Elsevier
• Subjects: Aglycones; Antioxidants; Antioxidants - analysis; Biological and medical sciences; Butylene Glycols - analysis; Butylene Glycols - metabolism; Chemical Fractionation; Chromatography, High Pressure Liquid; Chromatography, Liquid - methods; Extraction; Flax - chemistry; Flaxseed; gas chromatography; Gas Chromatography-Mass Spectrometry; GC/MS; General pharmacology; Glucosides - analysis; Glucosides - metabolism; high performance liquid chromatography; Hydrolysis; LC/MS; Least-Squares Analysis; Lignans; Lignans - analysis; Lignans - metabolism; linseed; mass spectrometry; Mass Spectrometry - methods; Medical sciences; Models, Chemical; Pharmacognosy. Homeopathy. Health food; Pharmacology. Drug treatments; Reproducibility of Results; Sensitivity and Specificity; Solid Phase Microextraction; Tandem Mass Spectrometry; time of flight mass spectrometry; Time-of-flight; Antioxidants; LC/MS; Hydrolysis; Flaxseed; MS; Aglycones; Lignans; Extraction; Time-of-flight; GC/MS; Solid phase extraction; Tandem mass spectrometry; Chemical analysis; Aglycone; HPLC chromatography; Solvent extraction; Fiber crop; Electrospray; Chemical enrichment; Medicinal plant; Acid hydrolysis; Linum usitatissimum; Sample preparation; Linaceae; Dicotyledones; Angiospermae; Lignan; Glycoside; Quantitative analysis; Liquid liquid extraction; Coupled method; Pharmacognosy; Linseed; Antioxidant; Gas chromatography; Time of flight method; Plant origin; Spermatophyta; Mass spectrometry; Comparative study
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2008.11.063

A new method of flaxseed-derived lignan determination was developed using HPLC with high-resolution time-of-flight MS (TOF-MS), optimized, and compared to two existing methods (HPLC/MS/MS and GC/MS). The limits of detection (LODs) for HPLC/TOF-MS (0.002–0.043 pg) were comparable with those of the optimized and improved HPLC/MS/MS (0.001–0.015 pg), whereas the LODs for the optimized GC/MS were higher (0.02–3.0 pg, yet lower than reported before). Using the newly developed detection and separation methods, several key flaxseed sample preparation parameters (including extraction, hydrolysis, and sample purification) were evaluated resulting in the development of efficient protocol for lignan quantification from flaxseed hulls and embryos. The results confirmed the importance of quantification of both aglycones and unhydrolyzed glucosides in order to obtain the total lignan estimates.