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Study On The Preparation And Quality Analysis Methods Of Flax Lecithin And Its Related Products

Posted on:2016-11-18Degree:MasterType:Thesis
Country:ChinaCandidate:Z L N E A E K GuFull Text:PDF
GTID:2191330479975706Subject:Analytical Chemistry
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Xinjiang is the main production base of agricultural and animal husbandry(the main province) in China. During the process of producing flax oil, the flax Oil residue and other by-products were also produced, which didn’t obtain good usage and development but were mostly regarded as waste, resulting in a waste of resources. The content of lecithin in Xinjiang flax oil residue was high, which can be comparable with that of soybean. In this research, the flax lecithin and relative products drived from flax oil residue were prepared and its quality analysis were performed. The main research content includes:First, in this research, the extraction technology with the flax lecithin were prepared.The flax oil residue at a pressure of 0.065~0.085 MPa, and vacuum dewatering concentrated phospholipid under the temperature of 80℃, and acetone deoiling, separation, drying to obtain raw phospholipids; Raw phospholipids at 55℃, 30 MPa conditions of supercritical fluid extraction, time is two hours. And by using column chromatography with silica gel as the adsorbent, take chloroform: methanol: water = 65:25:4(V/V/V) to elute separation and purification of lecithin, and its thinlayer chromatography analysis were performed. This method is convenient and fast.Secondly, prepared of lecithin liposome, lecithin compound and lecithin tablets by use flax lecithin and its quality analysis were performed. Based on single-factor experiments and orthogonal test, the optimal preparation conditions for flax lecithin liposome were determined to be chloroform as organic phase, p H=6.5 of PBS as aqueous phase, PC:Ch mass ratio of 4:1, the temperature was 40℃, An encapsulation efficiency of the flax lecithin liposome was 58.3%, and the average particle size of the flax lecithin liposome was 270 nm, the flax lecithin liposome stored in 4℃would keep stable. The optimized for lecithin compound were obtained as follows: the mass ratio of lecithin and quercetin was 1:2(g/g), the reaction time was 4 hours, the reaction temperature was 55℃, and its determination of melting point, ultraviolet and infrared spectrum to quality analysis were performed. From the four design of the prescription in lecithin tablet, screening of section three as the best program and its quality analysis results show that, in accordance with the requirements of the quality of the tablets.Thirdly, to establish a method for the quality analysis of lecithin extracted from flax by high performance thin layer chromatography(HPTLC). The effects of chromogenic agents, developing systems, amounts of spotted sample, thin layer chromatography plates, temperature and relative humidity on the separation of each component in sample were investigated. Screening the optimum separation conditions and its quality analysis were performed. The average content of phosphatidylcholine in flax lecithin sample was 63.33%with plate-to-plate and within-plate precision(relative standard deviation, RSD) of 1.8% and 3.7%, respectively, and stability(RSD) of 1.6%, and the average recovery was 98.5%. The results showed that, the method is rapid, accurate and reproducible, which can provide a new technical reference for the quality analysis of lecithin.Finally, to establish a method for the quality analysis of lecithin extracted from flax by high performance liquid chromatography(HPLC). A C18 column was used to determine the concentrations of three components in lecithin by HPLC, the mobile phase of methanol:acetonitrile:isopropanol(37:2:61, V:V:V), the wavelength of detector set at 206 nm, the flow rate was 1.0ml/min, the column temperature was 35℃ and injection volume was 10μl. The average content of PC、PI and LPC in lecithin sample was 57.69%、4.13%、13.38%, the precision RSD was 1.7%、2.9%、2.6% and the average recovery was100.7%、98.4% and 97.4%. The results show that the established method use for separation and analysis of PI、PC、LPC in lecithin. The method is simple, separation, accurate and separation effieciency.
Keywords/Search Tags:Lecithin, Flax Lecithin, Preparation Process, Quality Analysis
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