Knowledge Management System Of Institute of process engineering,CAS
一方面为了提高黑果枸杞食用的便利性、有效性并拓宽其应用范围，同时为了更深入地了解黑果枸杞及其相关产品花色苷的结构与功效，本研究采用超声提取、喷雾干燥技术制备黑果枸杞速溶粉，对制备的黑果枸杞速溶粉进行了品质评价、抗氧化活性测定以及改善动物睡眠实验，并探索了黑果枸杞花色苷的分离纯化工艺。 在单因素试验的基础上，采用正交试验优化黑果枸杞花色苷的超声辅助水提工艺，比较了热风干燥、超声干燥、冷冻干燥、喷雾干燥对提取物的干燥效果，采用响应面法优化了喷雾干燥工艺，并对所得速溶粉的微观形态、粒径大小、溶解时间等进行了表征与测量。结果表明：最佳提取工艺为超声功率400 W、料液比1:20（g/mL）、提取温度20℃、提取时间50 min；喷雾干燥最佳工艺参数为进风温度190℃、进样速度20 mL/min、料液密度1.01 g/cm3；喷雾干燥制备的黑果枸杞速溶粉粒径范围4~60 μm，平均粒径17 μm，平均完全溶解时间为43.4 s，达到了行业标准。 对黑果枸杞速溶粉的等级与营养成分进行了鉴定与分析，并测定了其体外抗氧化活性。所制备黑果枸杞速溶粉为一等品，含有17种氨基酸，其中天冬氨酸含量最高(1.345%)；并采用亚硝酸钠-硝酸铝法、香草醛-浓盐酸法、苯酚-硫酸法、pH示差法测定了速溶粉中黄酮、原花青素、多糖、花色苷的含量，分别为6.02%、2.88%、6.88%、1.40%。通过HPLC-DAD分析得出速溶粉中含有多种花色苷，其中有两种主要的花色苷为天竺葵素-3-O-二葡糖苷和天竺葵素-3-O葡萄糖苷。速溶粉具有较强的还原能力，能清除ABTS+·自由基、DPPH自由基，IC50分别为0.077 mg/mL、0.061 mg/mL，表现出良好的体外抗氧化活性。 采用萃取、大孔树脂、葡聚糖凝胶、半制备色谱等技术进行黑果枸杞花色苷的分离、纯化。通过静态吸附实验筛选出了AB-8型树脂，并通过动态吸附泄漏实验、动态洗脱实验确定了最佳上样体积(6 BV)、最佳洗脱条件(40%乙醇溶液)。将大孔树脂纯化后的样品经葡聚糖凝胶LH-20、半制备液相处理得到两个黑果枸杞花色苷单体。 研究了黑果枸杞速溶粉、黑果枸杞粗多糖、黑果枸杞粗多酚三个样品对小鼠睡眠的影响。虽然三个样品均对巴比妥钠诱导小鼠睡眠时间无显著影响，但可减少小鼠自主活动次数、降低小鼠血清MDA水平、升高SOD活性， 其中黑果枸杞粗多酚能够缩短小鼠睡眠潜伏期。 ;In order to increase the convenience and efficiency of using Lycium ruthenicum Murr and to broaden its application, Lycium ruthenicum Murr instant powder was prepared by ultrasonic-assisted extraction and spray drying technique. Then its quality, antioxidant activity and sleep improvement were studied. In addition, to learn more knowledge about the structure and function of anthocyanins from Lycium Ruthenicum Murr and its related product, anthocyanins purification process was studied.The extraction process was optimized through orthogonal test. The methods to dry Lycium ruthenicum Murr aqueous extract (hot air drying, ultrasonic drying, freeze drying and spray drying) were compared. Spray drying process was optimized by using response surface method. In addition, the micro morphology, particle size, and dissolution time of the obtained instant powder were studied. Ultrasonic extraction results showed that the optimal extraction conditions were as follows: ultrasonic power 400 W, solid-to-solvent ratio 1:20 (g/mL), extraction temperature 20℃, extraction time 50 min. The optimal spray drying technological parameters were 190℃, 20 mL/min and 1.01 for inlet air temperature, inject speed and liquor density, respectively. the range of size distribution of Lycium ruthenicum Murr powder produced by spray drying was 4 ~60 μm and the mean particle size was 17 μm. The average dissolution time of instant powder was 43.4 s, which reached the industry standard.The grade, nutritive compositions and anti-oxidative activity in vitro of Lycium ruthenicum Murr instant powder were measured and analyzed. The instant powder is Grade A and 17 kinds of amino acids were determined with the highest concentration of aspartic acid (1.345%). The contents of total flavones, procyanidins, polysaccharide and anthocyanins in instant powder were measured using sodium nitrite - aluminum nitrate method, vanillin - concentrated hydrochloric acid method, phenol-sulfuric acid method and pH differential method. Results showed the contents were 6.02%, 2.88%, 6.88%, 2.88%, respectively. The HPLC-DAD analysis showed that there were a variety of anthocyanins in the instant powder, and two of the main anthocyanins were pelargonium- 3-o-diglycosides and the pelargonium-3-O glucoside. Instant powder had strong reducing power and can significantly eliminate ABTS+· free radicals and DPPH free radicals. In ABTS+· and DPPH radical scavenging assays, the free radical scavenging rate was 50% when Lycium ruthenicum Murr instant powder concentrations were 0.077 mg/mL ,0.061 mg/mL, respectively; These results support strong antioxidant activity in vitro for Lycium ruthenicum Murr instant powder.Extraction technology, macroporous resin, glucan gel and semi-preparative chromatography were used in the separation and purification of anthocyanin from Lycium ruthenicum Murr. After Lycium ruthenicum Murr water extract was extracted with ethyl acetate three times, the ethyl acetate phase was close to colorless. The best adsorption macroporous resin(AB-8), optimal sample volume (6 BV) and optimal eluent condition (40% ethanol solution) were determined by static adsorption experiment, dynamic adsorption leakage experiment and dynamic elution experiment, respectively. Two Lycium ruthenicum Murr anthocyanin monomers were obtained when the sample purified by AB-8 macroporous resin was processed by glucan gel LH-20 and semi - preparative liquid chromatography.The effects of Lycium ruthenicum Murr instant powder, Lycium ruthenicum Murr crude polysaccharide and Lycium ruthenicum Murr crude anthocyanins on the sleep quality of mouse were studied. The results showed that: the three samples had no significant effect on barbital sodium induced mice sleep time, but can reduce the number of autonomic activities of mouse; All three samples could reduce the serum MDA level and increase serum SOD activity of the mouse; The Lycium ruthenicum Murr crude anthocyanins could shorten the sleep latency of mouse.
|杨冬彦. 黑果枸杞速溶粉的制备及其品质评价[D]. 中国科学院大学,2018.|
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