短梗五加果花色苷的制备及其在可食性油墨中的应用

发布时间：2018-08-27 08:09

【摘要】：本文是国家科技支撑计划项目(编号：2015BAD16B00)“防腐保鲜新型物流包装材料开发”、吉林省科技发展计划项目(编号：20140520182JH)“长白山短梗五加浆果花色苷可食性油墨的基础研究”和吉林省教育厅规划项目(编号：吉教科合字[2014]第556号)“长白山刺五加浆果花色苷的提取、纯化及抗氧化功能的研究”的部分内容。长白山区短梗五加资源丰富，短梗五加果作为一种新型的药食同源食品开发利用较少，造成了资源的浪费。本文以短梗五加果为原料，主要对短梗五加果花色苷(AFA)的提取、纯化、冷冻干燥工艺、稳定性、微胶囊化、抗氧化活性及在可食性油墨中的应用等方面进行了研究，研究结果如下： (1)采用单因素试验、正交试验和响应面试验确定了溶剂法、超声波辅助法、酶法、超声波—微波协同法提取AFA的最佳工艺条件，并从提取率、提取时间、能耗等方面对四种方法进行比较。溶剂法的最佳工艺条件为：提取时间2h、pH为2、40%的乙醇、提取温度60℃、液料比10:1(mL:g)，提取率为78.5%；超声波辅助法的最佳工艺条件为：超声功率160W，超声时间40min，液料比10:1(mL:g)，pH为2、40%的乙醇为提取剂，提取温度60℃，提取率为80.7%；酶法的最佳工艺条件为：纤维素酶用量0.7%、液料比15:1(mL:g)、酶解时间120min，，酶解温度50℃，pH为5.0，提取率为79.1%；超声—微波协同法的最佳工艺条件为：超声功率120W，微波功率180W，提取时间6.7min，液料比为10:1(mL:g)、pH为2、40%的乙醇为提取剂，提取温度为50℃，提取率为83.4%。超声—微波协同法提取AFA具有提取率高、提取时间短、能耗低等优点。 (2)采用大孔树脂法纯化AFA，以吸附率和解吸率为考察指标，确定AFA的最佳纯化条件：AB-8型大孔树脂对AFA的静态吸附平衡时间为4h，静态解吸平衡时间为2h，上样液pH为2，洗脱液pH为2，洗脱液乙醇体积分数70%，上样流速1mL·min-1，质量浓度1mg·mL-1，洗脱液的流速1mL·min-1。采用单因素试验和响应面试验，以AFA干燥速率、总花色苷保留率和水分含量为考察指标，确定真空冷冻干燥AFA的最佳工艺条件：干燥压力50Pa，物料厚度8mm，加热板温度50℃，AFA的干燥速率、总花色苷保留率和水分含量分别为19.37g·(g·h)-1、82.88%、4.13%。定性实验结果表明：AFA是含有酚羟基、在5号位没有取代的黄酮类化合物，其成分中可能含有矢车菊素、牵牛花素和飞燕草素。 (3) AFA在pH"f3的条件下较稳定，对室外强光较敏感，在60℃以下较稳定，氧化剂对AFA影响较显著，还原剂对AFA影响不显著，K+、Ca2+和Mg2+对AFA无影响，Na+、Zn2+、Al3+和高浓度的Cu2+对AFA有增色作用，Fe3+和Fe2+对AFA影响显著，蔗糖和葡萄糖对AFA有增色的作用，山梨酸钾对AFA无影响，高浓度的抗坏血酸对AFA影响较大。 (4)采用单因素试验、响应面试验和正交试验确定了研磨法、锐孔法和喷雾干燥法微胶囊化AFA的最佳工艺条件，探讨了不同因素对包埋效率的影响。研磨法最佳工艺条件为：壁芯比3.6:1、研磨时间43min、研磨温度40℃，包埋效率为76.4%，研磨法制备的短梗五加果花色苷微胶囊(AFAM)为松散、均匀细腻的粉末状，其微观结构呈球形，表面光滑、致密，无裂痕。锐孔法最佳工艺条件为：海藻酸钠质量分数1.9%、壳聚糖质量分数1.7%、氯化钙质量分数1%和壁芯比4:1，包埋效率为92.9%，锐孔法制备的AFAM呈球形，大小均匀，结构较完整、致密，有一定的机械强度，表面无裂痕。喷雾干燥法最佳工艺条件为：壁芯比6:1、固形物含量30%、麦芽糊精/阿拉伯胶1:1、进风口温度160℃、出风口温度80℃，包埋效率为83.3%，喷雾干燥法制备AFAM为均匀、细腻、松散的粉状，其微观结构呈较规则球形，表面光滑、致密，无裂痕。喷雾干燥法制备AFAM对温度、光照、pH和金属离子等因素都有较好的稳定性，在模拟胃液中有一定的缓释效果。 (5) AFA对DPPH自由基的清除效果显著，IC50为28.7ug/mL。AFA有一定的超氧阴离子自由基清除作用，IC50为134.1ug/mL。AFA对羟自由基的清除率较高，IC50为29.2ug/mL。AFA有较强的抗脂质过氧化能力，IC50为150.3ug/mL。AFA有一定的还原能力和抗油脂氧化能力。 (6)以1%的短梗五加果花色苷为色料，30%绵白糖、34.1%大豆油和34.1%蒸馏水为连接料，0.3%的黄原胶和0.5%卵磷脂为助剂，经超声-微波协同乳化20min制备短梗五加果花色苷可食性油墨，其粘度为0.32Pa s，流动度为37mm，细度㩳15um，经刮样纸检测，该油墨的面色与底色较接近，着色力较好，颜色鲜艳自然。L*值为44.62，a*值为24.44，b*值为15.43，彩度为28.90，色角为32.27°。采用丝网印刷将AFAEI印刷于面包表面、蛋糕表面和纸张上，图像清晰，色彩自然，有一定的装饰效果。AFAEI能耐受的最高干燥温度为70℃，有一定的耐酸性、耐乙醇性和耐水性，耐碱性较差，在实际应用中应避免接触碱性物质。Bloom测试和触变性测试的结果表明AFAEI基本性能与标准红墨较为接近。
[Abstract]:This paper is a project of National Science and Technology Support Program (No. 2015BAD16B00) "Development of New Logistics Packaging Materials for Preservation and Freshness Preservation", Jilin Province Science and Technology Development Program (No. 20140520182JH) "Basic Research on Anthocyanin Edible Ink of Acanthopanax senticosus Berries in Changbai Mountain" and Jilin Provincial Education Department (No. 2015BAD16B00). 2014] No. 556) "Extraction, Purification and Antioxidant Activity of Anthocyanins from Acanthopanax senticosus Berries in Changbai Mountain".
The resources of Acanthopanax senticosus in Changbai Mountains are abundant, and the exploitation and utilization of Acanthopanax senticosus as a new kind of medicinal and food homologous food is less, resulting in the waste of resources. The application of ink has been studied. The results are as follows:
(1) Single factor test, orthogonal test and response interview were used to determine the optimum extraction conditions of AFA by solvent method, ultrasonic-assisted method, enzymatic method and ultrasonic-microwave synergistic method, and four methods were compared in terms of extraction rate, extraction time and energy consumption. The optimum extraction conditions were as follows: ultrasonic power 160W, ultrasonic time 40 min, ratio of liquid to material 10:1 (mL:g), pH 2,40% ethanol as extracting agent, extraction temperature 60 C, extraction rate 80.7%; cellulase dosage 0.7%, ratio of liquid to material 15.7%. 1 (mL:g), enzymatic hydrolysis time 120 min, enzymatic hydrolysis temperature 50 C, pH 5.0, extraction rate 79.1%; ultrasonic-microwave synergistic method: ultrasonic power 120W, microwave power 180W, extraction time 6.7 min, liquid-to-material ratio 10:1 (mL: g), pH 2,40% ethanol as extractant, extraction temperature 50 C, extraction rate 83.4%. The extraction of AFA has the advantages of high extraction rate, short extraction time and low energy consumption.
(2) AFA was purified by macroporous resin, and the optimum purification conditions were determined according to the adsorption and desorption rates. The equilibrium time of AB-8 macroporous resin for AFA was 4 hours, the equilibrium time of static desorption was 2 hours, the pH of sample solution was 2, the pH of eluent was 2, the volume fraction of eluent was 70%, the flow rate of sample was 1 mL.min-1, and the mass concentration was 1 mg.m. L-1, eluent flow rate 1 mL The content of AFA was 19.37 g ((g h) - 1,82.88% and 4.13% respectively. The qualitative results showed that AFA was a kind of flavanone compound with phenolic hydroxyl group and no substitution at position 5. It may contain cyanidin, morning glory element and delphinidin.
(3) AFA is more stable under pH "f 3", more sensitive to outdoor strong light, more stable under 60 C, oxidant has a significant effect on AFA, reducing agent has no significant effect on AFA, K +, Ca2 + and Mg2 + have no effect on AFA, Na +, Zn2 +, Al3 + and high concentration of Cu2 + have a coloring effect on AFA, Fe3 + and Fe2 + have a significant effect on AFA, sucrose and glucose have a coloring effect on AFA. Potassium sorbate had no effect on AFA, and high concentration of ascorbic acid had great effect on AFA.
(4) The optimum technological conditions of microencapsulation of AFA by grinding method, sharp hole method and spray drying method were determined by single factor test, response interview test and orthogonal test, and the effects of different factors on the embedding efficiency were discussed. Anthocyanin microcapsules of Acanthopanax senticosus (AFAM) were prepared in a loose, uniform and fine powder form. The microstructure of the microcapsules was spherical, smooth, compact and crack-free. The optimum conditions of sharp-hole method were as follows: sodium alginate mass fraction 1.9%, chitosan mass fraction 1.7%, calcium chloride mass fraction 1% and Wall-Core ratio 4:1, embedding efficiency 92.9%, and sharp-hole method. The prepared AFAM is spherical, uniform in size, complete in structure, compact, with certain mechanical strength and no cracks on its surface. The optimum technological conditions of spray drying method are as follows: Wall-Core ratio 6:1, solid content 30%, maltodextrin/arabic gum 1:1, inlet temperature 160, outlet temperature 80, embedding efficiency 83.3%. The AFAM prepared by spray drying method is uniform and fine. Fatty, loose powder, its microstructure is more regular spherical, smooth surface, compact, no cracks. Spray drying AFAM prepared by temperature, light, pH and metal ions and other factors have a good stability, in simulated gastric juice has a certain slow-release effect.
(5) The scavenging effect of AFA on DPPH free radicals is remarkable. IC50 is 28.7ug/mL. AFA has a certain superoxide anion free radical scavenging effect, IC50 is 134.1ug/mL. AFA has a higher scavenging effect on hydroxyl free radicals, IC50 is 29.2ug/mL. AFA has a stronger anti-lipid peroxidation ability, IC50 is 150.3ug/mL. AFA has a certain reducing ability and anti-lipid oxidation ability.
(6) The edible anthocyanin ink of Acanthopanax senticosus was prepared by ultrasonic-microwave emulsification for 20 minutes with 1% anthocyanin as pigment, 30% sponge sugar, 34.1% soybean oil and 34.1% distilled water as binder, 0.3% xanthogen gum and 0.5% lecithin as auxiliaries. The viscosity, fluidity and fineness of the ink were 0.32 Pas, 37 mm and 15 um respectively. The color of the ink is close to the base color, and the color is bright and natural. L * value is 44.62, a * value is 24.44, b * value is 15.43, color is 28.90, color angle is 32.27 degrees. AFAEI is printed on the surface of bread, cake and paper by screen printing. The image is clear, the color is natural, and has a certain decorative effect. The highest drying temperature AFAEI can tolerate. The results of Bloom test and thixotropy test show that the basic properties of AFAEI are close to those of standard red ink.
【学位授予单位】：吉林大学
【学位级别】：博士
【学位授予年份】：2015
【分类号】：TS206.4

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