【摘要】：本文是國(guó)家科技支撐計(jì)劃項(xiàng)目(編號(hào)：2015BAD16B00)“防腐保鮮新型物流包裝材料開(kāi)發(fā)”、吉林省科技發(fā)展計(jì)劃項(xiàng)目(編號(hào)：20140520182JH)“長(zhǎng)白山短梗五加漿果花色苷可食性油墨的基礎(chǔ)研究”和吉林省教育廳規(guī)劃項(xiàng)目(編號(hào)：吉教科合字[2014]第556號(hào))“長(zhǎng)白山刺五加漿果花色苷的提取、純化及抗氧化功能的研究”的部分內(nèi)容。 長(zhǎng)白山區(qū)短梗五加資源豐富，短梗五加果作為一種新型的藥食同源食品開(kāi)發(fā)利用較少，造成了資源的浪費(fèi)。本文以短梗五加果為原料，主要對(duì)短梗五加果花色苷(AFA)的提取、純化、冷凍干燥工藝、穩(wěn)定性、微膠囊化、抗氧化活性及在可食性油墨中的應(yīng)用等方面進(jìn)行了研究，研究結(jié)果如下： (1)采用單因素試驗(yàn)、正交試驗(yàn)和響應(yīng)面試驗(yàn)確定了溶劑法、超聲波輔助法、酶法、超聲波—微波協(xié)同法提取AFA的最佳工藝條件，并從提取率、提取時(shí)間、能耗等方面對(duì)四種方法進(jìn)行比較。溶劑法的最佳工藝條件為：提取時(shí)間2h、pH為2、40%的乙醇、提取溫度60℃、液料比10:1(mL:g)，提取率為78.5%；超聲波輔助法的最佳工藝條件為：超聲功率160W，超聲時(shí)間40min，液料比10:1(mL:g)，pH為2、40%的乙醇為提取劑，提取溫度60℃，提取率為80.7%；酶法的最佳工藝條件為：纖維素酶用量0.7%、液料比15:1(mL:g)、酶解時(shí)間120min，，酶解溫度50℃，pH為5.0，提取率為79.1%；超聲—微波協(xié)同法的最佳工藝條件為：超聲功率120W，微波功率180W，提取時(shí)間6.7min，液料比為10:1(mL:g)、pH為2、40%的乙醇為提取劑，提取溫度為50℃，提取率為83.4%。超聲—微波協(xié)同法提取AFA具有提取率高、提取時(shí)間短、能耗低等優(yōu)點(diǎn)。 (2)采用大孔樹(shù)脂法純化AFA，以吸附率和解吸率為考察指標(biāo)，確定AFA的最佳純化條件：AB-8型大孔樹(shù)脂對(duì)AFA的靜態(tài)吸附平衡時(shí)間為4h，靜態(tài)解吸平衡時(shí)間為2h，上樣液pH為2，洗脫液pH為2，洗脫液乙醇體積分?jǐn)?shù)70%，上樣流速1mL·min-1，質(zhì)量濃度1mg·mL-1，洗脫液的流速1mL·min-1。采用單因素試驗(yàn)和響應(yīng)面試驗(yàn)，以AFA干燥速率、總花色苷保留率和水分含量為考察指標(biāo)，確定真空冷凍干燥AFA的最佳工藝條件：干燥壓力50Pa，物料厚度8mm，加熱板溫度50℃，AFA的干燥速率、總花色苷保留率和水分含量分別為19.37g·(g·h)-1、82.88%、4.13%。定性實(shí)驗(yàn)結(jié)果表明：AFA是含有酚羥基、在5號(hào)位沒(méi)有取代的黃酮類化合物，其成分中可能含有矢車菊素、牽�；ㄋ睾惋w燕草素。 (3) AFA在pH"f3的條件下較穩(wěn)定，對(duì)室外強(qiáng)光較敏感，在60℃以下較穩(wěn)定，氧化劑對(duì)AFA影響較顯著，還原劑對(duì)AFA影響不顯著，K+、Ca2+和Mg2+對(duì)AFA無(wú)影響，Na+、Zn2+、Al3+和高濃度的Cu2+對(duì)AFA有增色作用，F(xiàn)e3+和Fe2+對(duì)AFA影響顯著，蔗糖和葡萄糖對(duì)AFA有增色的作用，山梨酸鉀對(duì)AFA無(wú)影響，高濃度的抗壞血酸對(duì)AFA影響較大。 (4)采用單因素試驗(yàn)、響應(yīng)面試驗(yàn)和正交試驗(yàn)確定了研磨法、銳孔法和噴霧干燥法微膠囊化AFA的最佳工藝條件，探討了不同因素對(duì)包埋效率的影響。研磨法最佳工藝條件為：壁芯比3.6:1、研磨時(shí)間43min、研磨溫度40℃，包埋效率為76.4%，研磨法制備的短梗五加果花色苷微膠囊(AFAM)為松散、均勻細(xì)膩的粉末狀，其微觀結(jié)構(gòu)呈球形，表面光滑、致密，無(wú)裂痕。銳孔法最佳工藝條件為：海藻酸鈉質(zhì)量分?jǐn)?shù)1.9%、殼聚糖質(zhì)量分?jǐn)?shù)1.7%、氯化鈣質(zhì)量分?jǐn)?shù)1%和壁芯比4:1，包埋效率為92.9%，銳孔法制備的AFAM呈球形，大小均勻，結(jié)構(gòu)較完整、致密，有一定的機(jī)械強(qiáng)度，表面無(wú)裂痕。噴霧干燥法最佳工藝條件為：壁芯比6:1、固形物含量30%、麥芽糊精/阿拉伯膠1:1、進(jìn)風(fēng)口溫度160℃、出風(fēng)口溫度80℃，包埋效率為83.3%，噴霧干燥法制備AFAM為均勻、細(xì)膩、松散的粉狀，其微觀結(jié)構(gòu)呈較規(guī)則球形，表面光滑、致密，無(wú)裂痕。噴霧干燥法制備AFAM對(duì)溫度、光照、pH和金屬離子等因素都有較好的穩(wěn)定性，在模擬胃液中有一定的緩釋效果。 (5) AFA對(duì)DPPH自由基的清除效果顯著，IC50為28.7ug/mL。AFA有一定的超氧陰離子自由基清除作用，IC50為134.1ug/mL。AFA對(duì)羥自由基的清除率較高，IC50為29.2ug/mL。AFA有較強(qiáng)的抗脂質(zhì)過(guò)氧化能力，IC50為150.3ug/mL。AFA有一定的還原能力和抗油脂氧化能力。 (6)以1%的短梗五加果花色苷為色料，30%綿白糖、34.1%大豆油和34.1%蒸餾水為連接料，0.3%的黃原膠和0.5%卵磷脂為助劑，經(jīng)超聲-微波協(xié)同乳化20min制備短梗五加果花色苷可食性油墨，其粘度為0.32Pa s，流動(dòng)度為37mm，細(xì)度㩳15um，經(jīng)刮樣紙檢測(cè)，該油墨的面色與底色較接近，著色力較好，顏色鮮艷自然。L*值為44.62，a*值為24.44，b*值為15.43，彩度為28.90，色角為32.27°。采用絲網(wǎng)印刷將AFAEI印刷于面包表面、蛋糕表面和紙張上，圖像清晰，色彩自然，有一定的裝飾效果。AFAEI能耐受的最高干燥溫度為70℃，有一定的耐酸性、耐乙醇性和耐水性，耐堿性較差，在實(shí)際應(yīng)用中應(yīng)避免接觸堿性物質(zhì)。Bloom測(cè)試和觸變性測(cè)試的結(jié)果表明AFAEI基本性能與標(biāo)準(zhǔn)紅墨較為接近。
[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.
【學(xué)位授予單位】：吉林大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2015
【分類號(hào)】：TS206.4

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