高順式β-胡蘿卜素及納米結(jié)構(gòu)脂質(zhì)載體的制備
發(fā)布時間：2018-09-09 13:07
【摘要】：現(xiàn)有研究表明,9-順-β-胡蘿卜素具有比全反式異構(gòu)體更強的生理活性。一般食物原料中多含有全反式β-胡蘿卜素,只有鹽生杜氏藻中9-順式β-胡蘿卜素的占比可以達到40%左右,但鹽生杜氏藻價格昂貴,不利于大規(guī)模生產(chǎn)應用。因此,尋求一種以全反式β-胡蘿卜素為原料,高效制備高順式異構(gòu)體含量、特別是高9-順-β-胡蘿卜素含量的異構(gòu)化方法非常必要。另外,由于自身結(jié)構(gòu)的限制,β-胡蘿卜素幾乎不溶于水、穩(wěn)定性較差且生物利用度不高,作者嘗試通過制備β-胡蘿卜素-納米結(jié)構(gòu)脂質(zhì)載體(β-C-NLC),有效克服β-胡蘿卜素的使用缺陷,以方便其在水基食品中的應用。高9-順占比β-胡蘿卜素產(chǎn)品制備方法研究。以化學合成法生產(chǎn)的β-胡蘿卜素(全反式占比達96%,9-順式占比僅為0.15%)為原料,采用常規(guī)溶劑回流法做初步異構(gòu)化處理,利用液相-離子阱質(zhì)譜聯(lián)用儀(HPLC-APCI-MS)對異構(gòu)化處理后的產(chǎn)物進行測定,發(fā)現(xiàn)其主要成分為15-順式、13-順式、9,13-雙順式、全反式和9-順式等五種β-胡蘿卜素異構(gòu)體,證實該測定方法有效。在對比常規(guī)溶劑回流、高溫短時溶劑回流、碘摻雜二氧化鈦納米催化劑配合溶劑回流等異構(gòu)化工藝的基礎上,對碘摻雜二氧化鈦納米催化劑配合溶劑回流工藝進行單因素及正交試驗,優(yōu)選出制備高9-順占比β-胡蘿卜素異構(gòu)體的最優(yōu)條件為:β-胡蘿卜素溶解在乙酸乙酯中,底物濃度1 mg/m L,體系溫度75°C,時間105 min,催化劑用量1.1 mg/mg(基于β-胡蘿卜素),此時,9-順式β-胡蘿卜素異構(gòu)體相對含量達到25.31%,總順式異構(gòu)體的相對含量為47.41%。反應過程中β-胡蘿卜素的降解率為12.6%。該制備方法適用于高9-順式β-胡蘿卜素的制備,且工藝簡單,成本較低。關于儲藏條件對異構(gòu)化產(chǎn)品穩(wěn)定性影響的研究結(jié)果表明:在避光避氧低溫并添加適量的抗氧化劑的條件下儲藏,可大大減少異構(gòu)化產(chǎn)品的氧化降解,提高其穩(wěn)定性。β-胡蘿卜素-納米結(jié)構(gòu)脂質(zhì)載體制備工藝研究。通過高壓均質(zhì)法制備β-胡蘿卜素-納米結(jié)構(gòu)脂質(zhì)載體并確定了最佳制備條件:經(jīng)加熱的油相(分子蒸餾單甘酯和中長鏈甘油酯)與水相(吐溫80作為表面活性劑)混合,混合物在16000 rpm下剪切處理2 min,再在500 bar壓力下均質(zhì)3次,總脂質(zhì)濃度為9%(w/v),表面活性劑濃度為1.4%(w/v),固液脂比例為3:1(w/w)。在該條件下,β-C-NLC中β-胡蘿卜素的包封率達到95.64%,納米結(jié)構(gòu)脂質(zhì)載體體系中β-胡蘿卜素的含量達到2.9 mg/g,其平均粒徑為191 nm,多分散指數(shù)(PDI)約為0.2,載體體系具有良好的分散穩(wěn)定性。透射電鏡結(jié)果表明載體呈球形。探究了貯藏條件對β-C-NLC穩(wěn)定性的影響。結(jié)果表明在避光避氧,貯藏溫度為4°C且p H為3.5-7.5的條件下貯藏時,其粒徑變化小,分散體系穩(wěn)定性好,β-胡蘿卜素的降解率低,β-C-NLC的穩(wěn)定性得到一定程度的提高。
[Abstract]:The present studies have shown that 9-cis-尾-carotene has stronger physiological activity than all-trans isomers. Most of the food raw materials contain all-trans 尾 -carotene, only 9- cis-beta-carotene can reach about 40% in the halophytic Dunaliella, but the price of Dunaliella salina is expensive, which is not conducive to large-scale production and application. Therefore, it is necessary to find an efficient isomerization method using all-trans 尾 -carotene as raw material to prepare high cis isomer content, especially 9cis 尾 -carotene content. In addition, because of the restriction of its own structure, 尾 -carotene is almost insoluble in water, and its stability is poor and its bioavailability is not high. The authors try to overcome the defects of 尾 -carotene by preparing 尾 -carotene-nano-structure lipid carrier (尾 -C-NLC). In order to facilitate its application in water-based food. Study on preparation method of 尾-carotene with high 9-cis ratio. Using 尾 -carotene produced by chemical synthesis (all-trans ratio of Prida 96- 9- cis is only 0.15%) as raw material, conventional solvent reflux method was used for preliminary isomerization treatment. Five 尾 -carotene isomers were determined by liquid-ion trap mass spectrometry (HPLC-APCI-MS) after isomerization. It was found that the main components of the isomerization products were 15-cis-13-cis 13-cis, all-trans and 9- cis-isomers. It was proved that this method is effective for the determination of 尾 -carotene isomers. On the basis of comparing the isomerization processes such as conventional solvent reflux, high temperature and short time solvent reflux, iodine doped titanium dioxide nanocatalyst and solvent reflux, etc. A single factor and orthogonal experiment was carried out for the preparation of 尾 -carotene isomers with high 9-cis-ratio 尾 -carotene by using iodine doped titanium dioxide nano-catalyst and solvent reflux process. The optimum conditions were as follows: 尾 -carotene dissolved in ethyl acetate, and the optimum conditions were as follows: 尾 -carotene was dissolved in ethyl acetate, and 尾 -carotene was dissolved in ethyl acetate. The substrate concentration was 1 mg/m / L, the system temperature was 75 擄C, and the catalyst dosage of 105 min, was 1.1 mg/mg (based on 尾 -carotene). The relative content of 尾 -carotene isomer reached 25.31 and the relative content of total cis-isomer was 47.41%. The degradation rate of 尾-carotene was 12. 6% during the reaction. The method is suitable for the preparation of high 9-cis 尾 -carotene, and the process is simple and the cost is low. The study on the effect of storage conditions on the stability of isomerized products shows that the oxidative degradation of isomerized products can be greatly reduced when stored under the condition of avoiding light and avoiding oxygen and adding appropriate amount of antioxidants. The preparation process of 尾-carotene-nano structure lipid carrier was studied. The 尾 -carotene nanostructure lipid carrier was prepared by high pressure homogenization method and the optimum preparation conditions were determined: the mixture of heated oil phase (molecular distillation monoglyceride and medium-long chain glycerol ester) and water phase (Tween 80 as surfactant). The mixture was shearing at 16000 rpm for 2 min, and then homogenized for 3 times under 500 bar pressure. The total lipid concentration was 9% (w / v), surfactant concentration was 1.4% (w / v) and solid-liquid / lipid ratio was 3:1 (w / w). Under these conditions, the encapsulation efficiency of 尾 -carotene in 尾 -C-NLC was 95.64, and the content of 尾 -carotene in nano-structured lipid carrier system was 2.9 mg/g,. The average particle size of 尾 -carotene in the carrier system was nm, and the polydispersity index (PDI) was about 0.2. The carrier system had good dispersion stability. Transmission electron microscopy showed that the support was spherical. The effect of storage conditions on the stability of 尾-C-NLC was investigated. The results showed that when the storage temperature was 4 擄C and pH was 3.5-7.5, the particle size changed little, the dispersion system was stable, the degradation rate of 尾 -carotene was low, and the stability of 尾 -C-NLC was improved to some extent.
【學位授予單位】：江南大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TS201.2;TB383.1
本文編號：2232464
[Abstract]:The present studies have shown that 9-cis-尾-carotene has stronger physiological activity than all-trans isomers. Most of the food raw materials contain all-trans 尾 -carotene, only 9- cis-beta-carotene can reach about 40% in the halophytic Dunaliella, but the price of Dunaliella salina is expensive, which is not conducive to large-scale production and application. Therefore, it is necessary to find an efficient isomerization method using all-trans 尾 -carotene as raw material to prepare high cis isomer content, especially 9cis 尾 -carotene content. In addition, because of the restriction of its own structure, 尾 -carotene is almost insoluble in water, and its stability is poor and its bioavailability is not high. The authors try to overcome the defects of 尾 -carotene by preparing 尾 -carotene-nano-structure lipid carrier (尾 -C-NLC). In order to facilitate its application in water-based food. Study on preparation method of 尾-carotene with high 9-cis ratio. Using 尾 -carotene produced by chemical synthesis (all-trans ratio of Prida 96- 9- cis is only 0.15%) as raw material, conventional solvent reflux method was used for preliminary isomerization treatment. Five 尾 -carotene isomers were determined by liquid-ion trap mass spectrometry (HPLC-APCI-MS) after isomerization. It was found that the main components of the isomerization products were 15-cis-13-cis 13-cis, all-trans and 9- cis-isomers. It was proved that this method is effective for the determination of 尾 -carotene isomers. On the basis of comparing the isomerization processes such as conventional solvent reflux, high temperature and short time solvent reflux, iodine doped titanium dioxide nanocatalyst and solvent reflux, etc. A single factor and orthogonal experiment was carried out for the preparation of 尾 -carotene isomers with high 9-cis-ratio 尾 -carotene by using iodine doped titanium dioxide nano-catalyst and solvent reflux process. The optimum conditions were as follows: 尾 -carotene dissolved in ethyl acetate, and the optimum conditions were as follows: 尾 -carotene was dissolved in ethyl acetate, and 尾 -carotene was dissolved in ethyl acetate. The substrate concentration was 1 mg/m / L, the system temperature was 75 擄C, and the catalyst dosage of 105 min, was 1.1 mg/mg (based on 尾 -carotene). The relative content of 尾 -carotene isomer reached 25.31 and the relative content of total cis-isomer was 47.41%. The degradation rate of 尾-carotene was 12. 6% during the reaction. The method is suitable for the preparation of high 9-cis 尾 -carotene, and the process is simple and the cost is low. The study on the effect of storage conditions on the stability of isomerized products shows that the oxidative degradation of isomerized products can be greatly reduced when stored under the condition of avoiding light and avoiding oxygen and adding appropriate amount of antioxidants. The preparation process of 尾-carotene-nano structure lipid carrier was studied. The 尾 -carotene nanostructure lipid carrier was prepared by high pressure homogenization method and the optimum preparation conditions were determined: the mixture of heated oil phase (molecular distillation monoglyceride and medium-long chain glycerol ester) and water phase (Tween 80 as surfactant). The mixture was shearing at 16000 rpm for 2 min, and then homogenized for 3 times under 500 bar pressure. The total lipid concentration was 9% (w / v), surfactant concentration was 1.4% (w / v) and solid-liquid / lipid ratio was 3:1 (w / w). Under these conditions, the encapsulation efficiency of 尾 -carotene in 尾 -C-NLC was 95.64, and the content of 尾 -carotene in nano-structured lipid carrier system was 2.9 mg/g,. The average particle size of 尾 -carotene in the carrier system was nm, and the polydispersity index (PDI) was about 0.2. The carrier system had good dispersion stability. Transmission electron microscopy showed that the support was spherical. The effect of storage conditions on the stability of 尾-C-NLC was investigated. The results showed that when the storage temperature was 4 擄C and pH was 3.5-7.5, the particle size changed little, the dispersion system was stable, the degradation rate of 尾 -carotene was low, and the stability of 尾 -C-NLC was improved to some extent.
【學位授予單位】：江南大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TS201.2;TB383.1
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