Studies On Comprehensive Extraction Of Tocopherol, Phytosterol And Squalene From Soybean Oil Deodorizer Distillate

Soybean oil deodorizer distillate is a promising starting material for the manufacturing of tocopherols, phytosterols and squalene. In order to achieve comprehensive extraction of tocopherol, phytosterol and squalene from soybean oil deodorizer distillate. So, this article reports the study on extraction technology mainly. Besides a simple and accurate HPLC-DAD method has been developed for simultaneous determination of tocopherols(a-5 (β+y)-and 8-tocopherols), phytosterols (campesterol, P-sitosterol and stigmasterol) and squalene in vegetable oil deodorizer distillates (VODD). And the application and quality standard of the products are also studied. The results of the studies are listed as follows:1. The RP-HPLC-DAD method was developed for simultaneous determination of tocopherols (α-, (β+y)-,8-), phytosterols (campesterol, β-sitosterol, stigmasterol) and squalene in VODD. Chromatographic separation was performed on a C18 column with a gradient elution of mobile phase (methanol-water (98:2, v/v) and isopropanol) at a flow rate of 1.0 mL/min in 33 min at 30 "C. The method was efficient, accurate, and can be applied for the simultaneous analysis of the tocopherols, phytosterols and squalene in VODD.2. The studies on comprehensive extraction of tocopherol, phytosterol and squalene from soybean oil deodorizer distillate. Which are divided into the following parts:1) A modified saponification process:the sample was saponified by 0.020 Is mL/g (Is:saponification value) ethanolic solution of NaOH(1.5 mol/L) at 70℃ for 45 min. After saponification, ZnCl2 (1.6 mol/L,0.010 Is mL/g) was added over a period of fifteen minutes. The fatty acid zinc salt precipitated out at-18℃. The filtrate was extracted with hexane and washed by distilled water. Crude extracts of tocopherols, phytosterols and squalene were obtained after the extracted liquor was concentrated under vacuum. The purity of tocopherols of crude extracts was 51.27%, the ratio of extraction was 95.83%.2) The purification process of tocopherols:717 anion exchange resin as the stationary phase, absolute ethyl alcohol as the eluting solvent and ethanol solution with 5% acetic acid as the desorption solvent. The study on the static test of adsorption shows that 717 anion exchange resin adsorption was 419.0 mg/g to tocopherols, it has a good adsorption properties for tocopherols. The dynamic adsorption process of tocopherols, faint yellow and yellow liquid were collected and concentrated, tocopherol product was obtained. The content of tocopherol product was 72.13%, the recovery rate of tocopherol was 84.29%.3) Purification of phytosterols by crystallization:ratio of material to liquid was 1:3 (W/V). Add crude phytosterols material to ethyl alcohol at 50℃, stirring it until it dissolved, then cooling it to room temperature. Crystallization temperature was-5-5℃ and ripening time was 24h. The content phytosterol product was 89.28%, the recovery rate of phytosterol was 92.37% under the optimal reaction conditions. After re-crystallizing, the content phytosterol product can be above 95%, he recovery rate of phytosterolwas above 70%.4) The purification process of squalene:200-300 silica gel as the stationary phase, n-hexane as the eluting solvent, the eluting rate was 10 mL/min, ratio of material to dry silica gel was 1:20 (W/W). The fraction of high sualene concentration was collected and concentrated, The content of squalene product was 54.29%, the ratio of extraction was 86.91%.3. The design of product development processes and the establishment of quality standard:product development processes has been designed for industry with five products:50% natural vitamin E oil,70% natural vitamin E oil,90% phytosterols,20% squalene and 50% squalene. And the quality standard of the five products has been established. It can provide the theoretical guide for the producing processes.