The Extraction Of Perilla Crude Oil Rich In Phospholipids And The Preparation Of Phospholipids From Oil Residue

Perilla, a kind of annual herb, was approved to be one of the food and drug items byChinese Ministry of Health. Perilla oil is rich in α-linolenic acid, presumably,α-linolenic acidcontent in perilla phospholipids is high as well. At present, the major phospholipid product issoybean phospholipids, which is rich in oleic acid, but α-linolenic acid content is very low.Compared with soybean phospholipids, perilla phospholipids are rich in ω-3polyunsaturatedfatty acids, which can effectively improve the excess ω-6fatty acids in soybean phospholipids.Therefore, for the comprehensive utilization of perilla resources and functional perillaphospholipids, perilla seed was set as the raw material. This study focused on the preparation,purification and identification of powder phospholipids which is rich in ω-3polyunsaturatedfatty acid and high content phosphatidyl ethanolamine (PE).With perilla seeds as raw material, the method of pressing and leaching was used toextract crude perilla oil. The yield was26.84%and39.60%and the total phospholipidscontent of perilla crude oil was1.37mg/g and2.24mg/g respectively. Therefore, leachingmethod was more advantageous to the extraction of perilla crude oil and total phospholipids.At the same time, the oil content of perilla seeds oil was41.60%, which was far higher thanthat of soybean oil.Later, the best extraction craft was optimized through the response surface method basedon the single factor experiment and the best craft was as follows: the material liquid ratio(M:M, g:g)1:2.35, extraction temperature65℃, extracting time2.5h. Under the condition,oil yield of perilla seeds was39.80%and the total phospholipids content was2.26mg/g. Thecrude perilla oil was appeared to be yellow and transparent and it smelt special. Its acid valuewas2.51mg/g, peroxide value was5.28mL/g (0.01mol/L Na2S2O3), saponification valuewas192.1mg/g and iodine value was208.4g/100g. Through the method of gaschromatography, it showed that the content of the unsaturated fatty acid, which mainlyincluded alpha linolenic acid, linoleic acid, and oleic acid, was92.15%and the content ofα-linolenic acid reached to61.40%, so perilla oil was proved to be a rare source of alphalinolenic acid.Second, with perilla crude oil as raw material, concentrated phospholipid was obtainedby acid method to degum. The factor of acetone insolubles content of concentratedphospholipid was set as as the indicator to get the best process conditions through orthogonalexperiment and the best condition was as follows: water content4%, acid content0.30%,degumming time40min and degumming temperature65℃. With this condition, the acetoneinsolubles content of the concentrated phospholipid was65.1%.With concertrated phospholipid as raw material, using the method of acetone deoiling,powder phospholipid was extracted. The powder phospholipid yield and acetone insolublescontent were set as the indexs to investigate the the influence of material liquid ratio, deoilingtime, deoiling temperature and deoiling times on the process of powder phospholipid yield.After that, the best deoiling process was optimized by orthogonal experiment and the bestcraft was material liquid ratio (M:V, g:mL)1:8, deoiling temperature20℃, deoliing time20 min and deoiling for3times. The yield of powder phospholipids was66.3%and the acetoneinsolubles content of powder phospholipids was90.8%. Then, the fatty acid composition ofthe powder phospholipid was analyzed by the method of gas chromatography. It was shownthat the major compositions of the total fatty acids were polyunsaturated fatty acids,especially α-inolenic acid content (34.39%) and linoleic acid (17.33%).Then, the PE content of powder phospholipid was determined by high performanceliquid chromatography (HPLC) and external standard method. It showed that PE was themajor component. The content was23.11%.and yield was37.02%The method of silica gel column chromatography was utilized to purify powderphospholipid and prepare phosphatidyl ethanolamine(PE). When the sample weight was3.0g,the purity of PE was set as the evaluation index to investigate the the influence of elutionagent and elution velocity on the purity of PE. It showed that the best chromatography processwas chloroform: methanol (V:V, mL:mL)=0:1and elution velocity3.0mL/min. The PEpurity was62.25%and was2.69times of that in powder phospholipid.The method of HPLC-MS was utilized for the research on the identification of perillaPE molecular species. The results showed that there were nine PE molecular species and theywere16:0/18:3-PE,16:0/18:2-PE,16:0/18:1-PE,18:3/18:3-PE,18:2/18:3-PE,18:2/18:2-PE,18:1/18:3-PE,18:1/18:2-PE,18:1/18:1-PE respectively.