Study On Preparation Of Lin Zi Microcapsule

Perilla（Perilla frutescens L.Britt.）is an annual herb belonging to the genus Labiatae.Perilla seed is the fruit of perilla,which is rich in nutrients and fatty acids.It is a excellent source ofα-linolenic acid and has many activities such as hypolipidemic,anti-inflammatory,anti-tumor,antioxidant and so on.It was included in the Chinese Pharmacopoeia and the first batch of"medicine and food homology"list issued by the Ministry of Health of China.Rana chensinensis ovum is the major by-product of Oviductus Ranae in the production of Oviductus Ranae in Jilin Province.It contains rich functional nutrients,especially unsaturated fatty acids.Studies have shown that Rana chensinensis ovum oil（RCOO）has the effects of regulating blood lipids,weight loss,sedation and anti-anxiety.Because basic research is not enough to support development and application,Rana chensinensis ovum is usually treated cheaply as waste and have not been fully developed and utilized,resulting in a serious waste of Rana chensinensis resources.Previous studies found that the polyunsaturated fatty acids（PUFAs）in perilla seed oil（PSO）and RCOO could not meet the nutritional requirements ofω-6/ω-3 PUFAs ratio and the needs of other biological activities,and were not suitable to be used in health food alone.In order to improve the dietary ratio of two kinds of oil,PSO and RCOO were rationally proportioned and prepared into microcapsules.The wall material of microcapsule can protect oil from environmental impact,improve bioavailability and cover up bad smell,give full play to the respective advantages of perilla PSO and RCOO as plant extract oil and animal extract oil,and improve the comprehensive utilization of Rana chensinensis resources and promote the sustainable development of Rana chensinensis industry.This paper is divided into four parts.Firstly,PSO was extracted from perilla seed by supercritical CO₂ fluid extraction equipment.With the extraction rate of PSO as index by response surface test,the effects of three factors（extraction pressure（MPa）,extraction temperature（℃）and extraction time（h））on the extraction process were discussed.The composition and content of unsaturated fatty acids in PSO were analyzed by HPLC.The physicochemical properties of PSO were determined.The results showed that according to the response surface model,the supercritical CO₂extraction conditions of PSO were as follows:extraction pressure 28.60 MPa,extraction temperature 47.10℃,extraction time 3.72 h.The best extraction rate of PSO was 42.88%.The average error between actual value and predicted value was 0.02%.The main unsaturated fatty acids contained in PSO wereα-linolenic acid（ALA）and linoleic acid（LA）by HPLC,and the contents were 12.68 mg/g and 2.21 mg/g,respectively.The results of The physical and chemical properties of PSO were relative density:0.929 g/m L,iodide value:199.07 g/100 g,saponification value:193.77 mg/g,moisture and volatiles:0.07%,insoluble impurities:0.03%,acid value:1.78 mg/g,peroxidation value:0.05 g/100 g,and all the indexes met the quality standards of PSO,and the ratings could almost all meet the first-order standards with no odor of organic solvents.The scavenging rate of PSO to DPPH radical obtained by supercritical CO₂fluid extraction showed that PSO had obvious antioxidant activity.In the second part,the process parameters of microencapsulation of RCOO and PSO were explored and optimized.PSO and RCOO（Optimization of extraction process parameters by preliminary study in laboratory）were obtained by supercritical CO₂ fluid extraction.Lin Zi microcapsule were prepared by spray drying and gelatin and arabic gum were used as wall materials.Taking the entrapment efficiency of microcapsule as an index,the single factor test combined with orthogonal test was used to explore the influence of four factors,namely gelatin and acacia gum ratio,wall core ratio,spray drying peristaltic pump injection rate（m L/min）and air temperature（℃）,on the preparation process.Finally,the optimal preparation process parameters of Lin Zi microcapsules were obtained as follows:gelatin-Arabic ratio 1:1,wall-core ratio 3:1,peristaltic pump injection speed 6 m L/min,spray drying temperature 170℃.Through the verification test,under the optimal conditions,the entrapment efficiency of Lin Zi microcapsule is 85.28%,and the entrapment effect of the two oils is good,which meets the requirement of microcapsule encapsulation efficiency more than 80%in Chinese Pharmacopoeia 2020 edition.In the third part,the quality of Lin Zi microcapsule prepared with the optimum process parameters selected in the second part were evaluated.The experimental results showed that the entrapment efficiency of Lin Zi microcapsule was 85.28%,the water content was 0.68%,the loose density was 0.25 g/cm~3,the vibrating density was 0.41g/cm~3,the solubility was 61.37 g/100 g,the resting angle was 32.27°,and the peroxide value was 0.098 g/100 g,which met the requirements of production.The morphology and structure of the microcapsule were observed by Fourier transform infrared spectroscopy,microscope and SEM,and it was further confirmed that the encapsulation of the microcapsule was good.Finally,the scavenging rate of DPPH free radicals in Linzi microcapsule was investigated.The experimental results show that Linzi microcapsule can effectively scavenge DPPH free radicals,which indicated that it had antioxidant activity.Finally,the stability of Lin Zi microcapsule was investigated.The effect of different treatments（high temperature,humidity,and strong light irradiation test）on the Lin Zi microcapsule,and compared with the mixed oil of RCOO and PSO.the results showed that the stability of the microencapsulated core oil was greatly improved in the environment of high temperature,high humidity and strong light irradiation,the quality change decreased and the antioxidant capacity was improved.Generally speaking,Lin Zi microcapsule are suitable for storage in dry and shaded environment at room temperature.The results of accelerated stability test showed that the appearance of microcapsule had no obvious change,and the entrapment efficiency could meet the requirements of Pharmacopoeia as a whole,indicating that the preparation technology of Lin Zi microcapsule was reasonable and feasible.