Quantitative analysis of phylloquinone (vitamin k1) in soy bean oils by high-performance liquid chromatography

Analytical Determination of Phylloquinone (Vitamin K1) in Olive Oils. Comparison with Other Vegetable Oils

“…The different steps of sample preparation were often done under subdued daylight [19,21,29,37,47] because the PH was rapidly destroyed by both daylight and fluorescent light. Among these standard compounds, the most used was 2 0 ,3 0 dihydrophylloquinone while PH was used according to a standard addition method [20,36,42,48] or as an external standard. Internal standards (2 0 ,3 0 dihydrophylloquinone, menaquinone-4, K 1(25), 2 H 4 -phylloquinone) were added to sample prior to its preparation and whose choice depended on the detection technique.…”

“…Internal standards (2 0 ,3 0 dihydrophylloquinone, menaquinone-4, K 1(25), 2 H 4 -phylloquinone) were added to sample prior to its preparation and whose choice depended on the detection technique. In certain experimental procedures, an enzymatic hydrolysis [20,23,29,48] or a saponification of oil [38] were performed in a first step, but more frequently a direct oil solubilization was made in organic solvent as hexane [12,18,22,36,37] or solvent mixture (acetone/chloroform). [29] Gao and Ackman [23] advocated an internal standard method that was much faster and more accurate than an external standard or a standard addition method.…”

“…In certain experimental procedures, an enzymatic hydrolysis [20,23,29,48] or a saponification of oil [38] were performed in a first step, but more frequently a direct oil solubilization was made in organic solvent as hexane [12,18,22,36,37] or solvent mixture (acetone/chloroform). This purification was often realised on a Sep-Pak (SPE) silica cartridge [12,18,22,23,39,42,49] and little on alumina column [48] and sometimes by semi preparative HPLC on μPorasil column. The enzymatic digestion was carried on 0.25-0.50 g of oil sample using 1.00-1.25 g of lipase in 5-100 mL of phosphate buffer.…”

“…[5,41] Then, oil samples have been generally purified prior to chromatographic analysis to remove lipids that may interfere when detecting PH. [20,36,42,48] Results were difficult to compare because they were not all related to olive oils but to different vegetable oils or margarines and the HPLC detector was not the same. [19,21,37] The SPE extraction with silica cartridge was generally conducted in four steps: (i) a conditioning of the stationary phase by a wash of hexane or a mixture or hexane/diethyl ether (96:4, v/v); (ii) a loading of the sample frequently dissolved in hexane; (iii) washing (s) of the cartridge with hexane to eliminate the less polar lipids and the hydrocarbons; and (iv) and finally elution of the fraction containing PH with hexane/diethyl ether (96:4, v/v) or methanol/2-propanol/n-hexane (95:2.5:2.5, v/v/v) or hexane/ diisopropyl ether (90:10, v/v).…”

“…Three studies reported PH quantification in oils using UV detection [37,38,48] despite the low selectivity and sensibility of this detector. Non-aqueous solvents were used with UV detection.…”