CN107996931B - 一种抗菌、强心护肝富氢低糖保健饮料及其制备方法 - Google Patents
一种抗菌、强心护肝富氢低糖保健饮料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种抗菌、强心护肝富氢低糖保健饮料及其制备方法,它由以下重量配比的原料制得:将马铃薯皮渣黄酮0.5~0.8g、玉米须酚酸0.2~0.5g、玉米芯低聚木糖0.5~2.0g、蒲公英根部含水乙醚提取物0.1~0.5g、冬虫夏草活性多肽0.05~0.1g以及藏红花乙醇提取物0.05~0.1g合并,以纯净水100mL配置成天然饮料原浆后,加入交联马铃薯淀粉0.2~0.4g制备天然抑菌淀粉乳溶液,将上述经震荡混合后的原浆溶液经低速均质法处理获得匀浆液,经水力喷射泵的文丘里结构,使其与0.50~0.60mL氢气充分混合,制备成保健饮料,产品中不添加防腐剂、增香剂、增稠剂等人工合成的添加剂。采用本发明制备的功能性保健饮料天然抑菌、功能突出,适宜于大众尤其适宜于高血糖、心脏病及肝脏欠佳的群体。
Description
技术领域
本发明涉及饮料生产技术领域,具体涉及一种抗菌、强心护肝富氢低糖保健饮料及其制备方法。
背景技术
当今社会,随着人民生活水平普遍提高,“富贵病”的发病率明显上升,一些以预防为主的功能性食品也崭露头角,在市场上的地位越来越重要。复合保健饮料的开发也呈现出生机勃勃的发展趋势,各种保健饮料层出不穷,各有千秋。在众多保健饮料中,补钙、延缓衰老、抗疲劳、增加免疫等系列产品较多,然而具有抗菌、强心护肝富氢低糖保健饮料却寥寥无几,难以满足心脏病及肝脏欠佳人群的需要。另外,市售大多数的饮料成分中均含有防腐剂、香精、增稠剂等,长期饮用,存在潜在的危害。
发明内容
本发明的目的在于提供一种采用纯天然原料制成,无任何添加剂及安全隐患,具有抗菌、强心、护肝、抗氧化等多种保健功能低糖饮料,以促进人体健康,丰富人们的需求,本发明还提供了制备方法。
为实现上述目的,本发明一种抗菌、强心护肝富氢低糖保健饮料,其原料及重量配比如下:交联马铃薯淀粉:0.2~0.4g、马铃薯皮渣黄酮:0.5~0.8g、玉米须酚酸:0.2~0.5g、玉米芯低聚木糖:0.5~2.0g、蒲公英根部含水乙醚提取物:0.1~0.5g、冬虫夏草活性多肽:0.05~0.1g、藏红花乙醇提取物:0.05~0.1g、氢气:0.50~0.60 mL、水100mL。
主要原料的功能特性如下:
马铃薯皮渣黄酮:马铃薯进行深加工时,大部分马铃薯皮渣作为废弃物丢弃,而马铃薯表皮及邻近组织含有丰富的黄酮类物质,具有抗氧化、抗病毒、保肝利胆、降血压、降血脂、调节免疫等功能,此外还是较好的天然抑菌剂;
玉米须酚酸:玉米须是玉米的干燥花丝和柱头,玉米须中含有的酚酸具有抗菌、抗炎、抗病毒、抗肿瘤、抗氧化、保肝等作用;
玉米芯低聚木糖:玉米芯作为玉米生产的副产物,通常被作为燃料而烧掉,不仅浪费资源还污染环境。玉米芯中含有的木聚糖可以降解产生低聚木糖。低聚木糖能促进肠道内益生菌的增殖,有益于肠道健康,甜度比蔗糖和葡萄糖均低,具有抗龋齿作用,是一种功能性食品基料;
蒲公英根部含水乙醚提取物:蒲公英根部的脂溶性成分和水溶性多糖具有抗菌、抗氧化、保肝利胆、抗肿瘤等功效;
冬虫夏草活性多肽:虫草多肽是虫草子实体蛋白经水解得到,分子量小,易吸收、起效快,具有扩张心脑血管、保护心肌细胞、肝脏细胞、提高免疫力,抗氧化、抑制多种致病菌等生理功能;
藏红花乙醇提取物:藏红花乙醇提取物的主要成分是藏红花苷类物质、类胡萝卜素以及番茄红素等,具有防治心血管疾病、抗氧化、提高免疫力、保肝护肾等生理功能。
本发明一种上述保健饮料的制备方法,包括如下具体步骤:
1.交联马铃薯淀粉的制备方法:取淀粉含量82%以上的马铃薯淀粉以1:2(g:mL)加水调浆后,在超声强度为180-200W,超声温度25℃条件下超声活化100min后,用1mol/LNaOH溶液调节至pH10.0,并将其置于37℃水浴锅中,缓慢少量多次加入一氯乙酸钠,即每15min加入用量为0.3%-0.4%的一氯乙酸钠,中间间隔5min,分四次加完,一氯乙酸钠的总用量为1.2%-1.6%,用电动搅拌器不断搅拌使淀粉发生交联,反应结束后,经盐酸中和至pH 6-7,蒸馏水洗涤三次,4000r/min离心20min,沉淀置于真空度≥0.09MPa,50℃真空干燥箱干燥8h,粉碎过60目筛,得交联马铃薯淀粉;
2.马铃薯皮渣黄酮的制备方法:将皮层厚度为0.15-0.5mm的马铃薯皮置于不锈钢托盘中铺平,放入50℃真空干燥箱中,真空干燥5h后,以万能粉碎机粉碎过60目筛备用。采用超高压梯度升压技术,按料液比1:10(g:mL)加入45%-55%的乙醇溶液,100MPa高压下浸提10-20min后,将压力提升至200MPa,5-10min后再提升至300MPa,超高压提取总时间20-40min,3500r/min离心20min后,将沉淀物以1:5(g:mL)加入45% 的乙醇溶液采用超声联合两步醇提技术,于超声功率为150-200W,超声温度为25℃条件下复提20min,合并两次滤液,减压浓缩后,得到的马铃薯皮渣黄酮粗提液与大孔吸附树脂AB-8以50:1(mL:g)混合后摇床中振荡吸附24 h,滤去未吸附溶液,再以1:25(g:mL)加入70%乙醇溶液继续于摇床振荡洗脱4-6h,离心过滤得滤液,减压浓缩后置超低温冰箱-70~-80℃冷冻12h,再由真空冷冻干燥机冷冻干燥10h得马铃薯皮渣黄酮;
3.玉米须酚酸的制备方法:取玉米须低温长时烘干后,将粉碎好的玉米须按1:1(g: mL)加入70%-90%乙醇夹带剂,将其再装入二氧化碳超临界浸提反应釜中,置于超声功率180-200W,超声温度50-60℃的超声清洗设备之中,开启二氧化碳进气阀与排气阀,设置反应压力250bar,出口阀温度100℃,排气1min后关闭排气阀,待超声反应容器与浸提反应釜温度平衡后,开启超声,二氧化碳静态联合超声浸提10-15min后关闭超声功率;然后进行动态萃取,二氧化碳流量2.5L/h,萃取时间15-25min,将上述静态动态萃取模式往复3次,得玉米须酚酸提取液。将得到的提取液采用动态吸附洗脱方式进行纯化,取一定量大孔吸附树脂XDA-1装柱,将玉米须酚酸提取液上样后,用60%乙醇溶液以2BV/h的流速进行洗脱,并于327nm处进行峰值检测,以自动组份收集仪收集出峰时间段对应的洗脱溶液,并减压浓缩,低温冰箱-70~-80℃冷冻12h,真空冷冻干燥10h得玉米须酚酸成品;
4.玉米芯低聚木糖的制备方法:将玉米芯与0.3mol/L的NaOH溶液按料液比1:25(g:mL)混合,在微波功率为480-600W,间歇式封闭微波辅助处理8-10min后,60℃水浴热提30min,3500r/min 条件下离心30min取上清液用0.1mol/L盐酸中和,加入3倍体积95%的乙醇沉淀;再于3500r/min条件下离心30min取沉淀,经氮气吹干得木聚糖粗品。将木聚糖粗品用pH5.0的柠檬酸缓冲液配置成4.0%-5.0%的溶液,添加底物1.0%的木聚糖酶(3,0000 U/g)于蒸煮袋中密封。将其放入超高压设备中,设置反应温度50℃,反应压力200MP,反应时间5-10min后,将温度提升至60℃,反应压力升至300MP,继续反应15-20min后取出沸水浴灭酶10min,再于3500r/min条件下离心20min得低聚木糖溶液。低温冰箱-70~-80℃冷冻12h,真空冷冻干燥10h得低聚木糖干粉。将冻干的低聚木糖干粉经超微粉碎设备进行粉碎细化,使其粒度范围D50<1μm;
5.蒲公英根部含水乙醚提取物的制备方法:将6-7月份采撷的蒲公英全草摘除叶片部分,45°角斜切斩断至1-2mm厚的根片,至瓦片上于电炉文火焙干,并以万能粉碎机粉碎过60目筛备用。以1:10(g:mL)加入2%饱和的含水乙醚为提取剂,采用索氏提取的回流装置,于35℃浸提回流3-4h,回收多余的乙醚,得初提液,经氮吹仪,控制分压表于0.3-0.4MPa,氮吹直至膏状变干,吹走残留乙醚。再分别以1:4,1:3和1:2的比例加入95%乙醇溶解、洗涤上述膏状物,并再次减压浓缩至膏状,反复操作三次。将膏状物置超低温冰箱-70~-80℃冷冻24h,再由真空冷冻干燥机冷冻干燥10h得配方原料;
6.冬虫夏草活性多肽的制备方法:取野生冬虫夏草干制品,适量喷淋纯净水,使其吸水润涨,并置于-76℃超低温冰箱急速冻结后,于冷冻粉碎机粉碎过60目筛备用。将粉碎后的样品以1:10(g:mL)加入缓冲溶液(0.02M,pH 7.5 PBS)为提取剂,置于微波-紫外-超声三位一体浸提设备中,微波输出功率360W,输出形式每间隔60s微波加热一次,同时超声工作频率26KHz,输出功率180W提取10-15min后,超声工作频率变为27KHz,输出功率180W再提取10-15min后,工作频率28KHz,输出功率不变,再提取10-15min,完成变频提取。将上述提取液置于真空冷冻干燥设备冷井-70~-80℃,8-10h完后冻结后,开启真空程序,进行冷冻浓缩,至蛋白含量为5.0%时,完成浓缩程序。将上述5.0%的蛋白溶液中加入3%-5%的胰蛋白复合酶(酶活4000U/g)充分混合后,装入聚乙烯塑料中,置于超高静压反应釜中,设置温度50℃,于超高压200MPa条件下酶解反应3-4h。将上述超高压联动酶解液于3500r/min离心10min取上清液,接入切向流超滤膜过滤系统,选用4000Da范围内分子膜对其过滤,从而获得特定区段的功能性虫草肽蛋白液。将蛋白液置超低温冰箱-70~-80℃冷冻24h,再由真空冷冻干燥机冷冻干燥10h得配方原料;
7.藏红花乙醇提取物的制备方法:取藏红花干制品,加入0.8%-1.2%的复合酶(含纤维素酶(10, 000 U/g)、半纤维素酶(10, 000 U/g)、β-葡萄糖苷酶(5, 000U/g)),按照料液比1:1.5(g:mL)加入50%的乙醇溶液,将其与物料调制成粘稠状,以尽可能快的方式转移至超临界萃取釜中,设定超临界反应釜反应压力300 bar,反应温度50℃、静压酶解时间3-4h,实现静态酶解提取阶段;结束后,打开排气阀,设置二氧化碳流量1.5 L/h进行动态超临界酶解萃取1-2 h,实现动态酶解提取阶段,获得提取液。将提取液至旋转蒸发仪上减压浓缩至膏状。将膏状提取物置于真空冷冻干燥设备冷井-70~-80℃,8-10h完后冻结后,开启真空程序,进行真空冷冻干燥10h,获得配方原料;
8.氢气的制备方法:以满足色谱仪的高纯氢气发生器为气体源,每分钟最大流量300mL,并可控得配方原料;
9.按照配方比例,合并0.5~0.8g马铃薯皮渣黄酮、0.2~0.5g玉米须酚酸、0.5~2.0g玉米芯低聚木糖、0.1~0.5g蒲公英根部含水乙醚提取物、0.05~0.1g冬虫夏草活性多肽以及0.05~0.1g藏红花乙醇提取物,且以纯净水100 mL配置成天然饮料原浆后,加入0.2~0.4g交联马铃薯淀粉制备天然抑菌淀粉乳溶液,于0-4℃低温水浴,振荡器转速100r/min条件下震荡2-3h,将上述经震荡混合后的天然饮料原浆溶液经85℃水浴糊化并不断搅拌,30-40min后停止搅拌保温孵化20-30 min,再低速搅拌条件下缓慢降至室温,以实现缓慢溶合,将上述溶合好的基料,以德国IKA T18内剪切均浆机以3500-4000rpm低速均质法处理获得匀浆液;
10.将上述匀浆液冷却后经水力喷射泵的文丘里结构,使其与0.50~0.60mL氢气充分混合接触,具体操作为:将氢气源流量设置为<60 mL/min,完全依靠文丘里气水混合结构,充分自然交溶,实现富氢功能保健饮料成品。多余氢气自然排出并引入大气,最终制备成富氢保健饮料成品。
所述水力喷射泵包括:泵体及泵体上设置的进气口、饮料浆液进口和成品饮料出口。
本发明的抗菌、强心护肝富氢低糖保健饮料,不仅拥有马铃薯皮渣黄酮、玉米须酚酸、蒲公英根部乙醚提取物、冬虫夏草活性多肽以及藏红花乙醇提取物多种物质的营养成分和保健功能,而且加入的玉米芯低聚木糖有益于肠道健康,甜度比蔗糖和葡萄糖均低,具有抗龋齿作用,同时,加入氢气的水具有很强的还原功能,可以中和身体血液和细胞里的活性氧(自由基),平衡身体酸碱度,有效防止多种疾病。另外本发明使用的马铃薯皮渣黄酮、玉米须酚酸、蒲公英根部含水乙醚提取物以及冬虫夏草活性多肽还是纯天然生物抗菌剂。产品中不添加任何防腐剂、增香剂、增稠剂等人工合成的添加剂。在生产工艺上采用先进的现代化仪器设备,做到省时、快捷、绿色。采用本发明制备的饮料天然抑菌、功能突出,是一种适宜于大众尤其适宜于高血糖、心脏病及肝脏欠佳群体的功能性保健饮料。
下面结合附图对本发明专用水力喷射泵作详细说明。
附图说明:
图1为本发明专用水力喷射泵主视图。
具体实施方式
实施例1 按照下列步骤制备本发明的富氢保健饮料:
1.交联马铃薯淀粉的制备:取淀粉含量82%以上的马铃薯淀粉100g,加入200mL水调浆后,在25℃超声活化,超声功率为180W,为避免超声时温度升高,采取间歇超声形式,即每隔15min超声10min,总计时间100min。超声活化后,用1mol/L NaOH溶液调节至pH10.0,将其置于37℃水浴锅中,缓慢少量多次加入一氯乙酸钠,即每15min加入0.3 g一氯乙酸钠,中间间隔5min,分四次加完,一氯乙酸钠的总用量为1.2g,期间用电动搅拌器不断搅拌使淀粉发生交联,反应结束后,经盐酸中和至pH 6.5,蒸馏水洗涤三次,4000r/min离心20min,沉淀置于真空度≥0.09MPa,50℃真空干燥箱干燥8h,粉碎过60目筛,得交联马铃薯淀粉;
2.马铃薯皮渣黄酮的制备:将皮层厚度为0.15-0.5mm的马铃薯皮置于不锈钢托盘中铺平,放入50℃真空干燥箱中,真空干燥5h后,以万能粉碎机粉碎过60目筛备用。取粉碎后的马铃薯皮渣100g,加入45%的乙醇溶液1000mL,100MPa高压下浸提15min后,将压力提升至200MPa,5min后再提升至300MPa,超高压提取总时间30min,3500r/min离心20min后,将沉淀物加100mL 45% 的乙醇溶液,于超声功率150W,25℃条件下复提20min,合并两次滤液,减压浓缩得马铃薯皮渣黄酮粗提液。100mL粗提液与2g大孔吸附树脂AB-8混合后摇床中振荡吸附24h,滤去未吸附溶液,树脂中加入70%乙醇溶液50mL继续于摇床振荡洗脱4h,离心过滤得滤液,减压浓缩后置超低温冰箱-70℃冷冻12h,再由真空冷冻干燥机干燥10h得马铃薯皮渣黄酮;
3.玉米须酚酸的制备:将玉米须低温长时烘干后,取粉碎后的玉米须50g,与50mL70%的乙醇夹带剂一并装入二氧化碳超临界浸提反应釜中,并将釜置于超声功率180W,超声温度50℃的超声清洗设备中,开启二氧化碳进气阀与排气阀,设置釜内压力250bar,出口阀温度100℃,排气1min后关闭排气阀,待超声反应容器与浸提反应釜温度平衡后,开启超声,二氧化碳静态联合超声浸提10min后关闭超声;然后进行二氧化碳动态超临界萃取,二氧化碳流量为2.5L/h,萃取时间为15min,将上述静态动态萃取模式往复3次,得玉米须酚酸提取液。将得到的玉米须酚酸提取液通过大孔吸附树脂XDA-1进行纯化,用60%乙醇溶液以2BV/h的流速进行洗脱,并于327nm处进行峰值检测,以自动组份收集仪收集出峰时间段对应的洗脱溶液,并减压浓缩,低温冰箱-70℃冷冻12h,真空冷冻干燥10h得玉米须酚酸成品;
4.玉米芯低聚木糖的制备:玉米芯50g与0.3mol/LNaOH溶液1250mL混合,在微波功率为480W,间歇式封闭微波辅助处理8min后,60℃水浴热提30min,3500r/min 条件下离心30min取上清液,用0.1mol/L盐酸中和后,取液体500mL,加1500mL95%乙醇沉淀;再于3500r/min条件下离心30min取沉淀,经氮气吹干得木聚糖粗品。将木聚糖粗品10g加入250mLpH5.0的柠檬酸缓冲液,添加0.1g木聚糖酶(3,0000 U/g)于蒸煮袋中密封。将其放入超高压设备中,设置反应温度50℃,反应压力200MP,反应时间5min后,将温度提升至60℃,反应压力升至300MP,继续反应15min后取出沸水浴灭酶10min,再于3500r/min条件下离心20min得低聚木糖溶液。低温冰箱-70℃冷冻12h,真空冷冻干燥10h得低聚木糖干粉。将冻干的低聚木糖干粉经超微粉碎设备进行粉碎细化,使其粒度范围D50<1 μm;
5.蒲公英根部含水乙醚提取物的制备:将6-7月份采撷的蒲公英全草摘除叶片部分,45°角斜切斩断至1-2mm厚的根片,至瓦片上于电炉文火焙干,并以万能粉碎机粉碎过60目筛备用。取粉碎后的蒲公英根10g,加入2%饱和的含水乙醚100mL,采用索氏提取的回流装置,于35℃浸提回流3h,回收多余的乙醚,得初提液,经氮吹仪,控制分压表于0.3MPa,氮吹直至膏状变干,吹走残留乙醚。取5g沉淀,分别以95%乙醇20mL、15mL以及10mL溶解、洗涤上述膏状物,并再次减压浓缩至膏状,反复操作三次。将膏状物置超低温冰箱-80℃冷冻24 h,再由真空冷冻干燥机冷冻干燥10h得配方原料;
6.冬虫夏草活性多肽的制备:取野生冬虫夏草干制品,适量喷淋纯净水,使其吸水润涨,并置于-76℃超低温冰箱急速冻结后,于冷冻粉碎机粉碎过60目筛备用。取粉碎后的样品10g加入100mL 0.02 mol/L pH 7.5的磷酸盐缓冲液,置于微波-紫外-超声三位一体浸提设备中,微波输出功率360W,输出形式每间隔60s微波加热一次,同时超声工作频率26KHz,输出功率180W提取10min后,超声工作频率变为27KHz,输出功率180W再提取10min后,工作频率28KHz,输出功率不变,再提取10min,完成变频提取。将上述提取液置于真空冷冻干燥设备冷井-70℃,8h完成冻结后,开启真空程序,进行冷冻浓缩,至蛋白含量为5.0%时,完成浓缩程序。取上述5.0%的蛋白溶液20mL,加入0.03g的胰蛋白复合酶(酶活4000 U/g)充分混合后,装入聚乙烯塑料中,置于超高静压反应釜中,设置温度50℃,于超高压200MPa条件下酶解反应3h。将上述超高压联动酶解液于3500r/min离心10min取上清液,接入切向流超滤膜过滤系统,选用4000Da范围内分子膜对其过滤,从而获得特定区段的功能性虫草肽蛋白液。将蛋白液置超低温冰箱-80℃冷冻24h,再由真空冷冻干燥机冷冻干燥10h得配方原料;
7.藏红花乙醇提取物的制备:取藏红花干制品5g,加入0.04g复合酶(含纤维素酶(10, 000 U/g)、半纤维素酶(10, 000 U/g)、β-葡萄糖苷酶(5, 000U/g)),再加入50%的乙醇7.5mL,将其与物料调制成粘稠状,以尽可能快的方式转移至超临界萃取釜中,设定压力300bar,反应温度50℃、静压酶解时间3h,结束后,打开排气阀,设置二氧化碳流量1.5L/h进行动态超临界酶解萃取1h,获得提取液。将提取液至旋转蒸发仪上减压浓缩至膏状。将膏状提取物置于真空冷冻干燥设备冷井-79℃,10h完后冻结,开启真空程序,进行真空冷冻干燥10h,获得配方原料;
8.氢气的制备:以满足色谱仪的高纯氢气发生器为气体源,每分钟最大流量300mL,获得配方原料;
9.将所得马铃薯皮渣黄酮0.5g、玉米须酚酸0.2g、玉米芯低聚木糖0.5g、蒲公英根部含水乙醚提取物0.1g、冬虫夏草活性多肽0.05g以及藏红花乙醇提取物0.05g,加入100mL纯净水,配置成天然饮料原浆后,加入0.4g交联马铃薯淀粉制备天然抑菌淀粉乳溶液,于4℃低温水浴,振荡器转速100r/min条件下震荡3h。将上述经震荡混合后的天然饮料原浆溶液经85℃水浴糊化并不断搅拌,40min后停止搅拌保温孵化20min,再低速搅拌缓慢降至室温,以实现缓慢溶合。将上述溶合好的基料,以德国IKA T18内剪切均浆机以3500rpm低速均质法处理获得匀浆液;
10、将得到的匀浆液经水力喷射泵的文丘里结构,使其与0.5mL的氢气充分混合接触,氢气源流量设置为60mL/min,完全依靠文丘里气水混合结构,充分自然交溶,实现富氢功能保健饮料成品。多余氢气自然排出并引入大气,最终制备成富氢保健饮料成品。
所述水力喷射泵包括:泵体及泵体上设置的进气口A、饮料浆液进口B和成品饮料出口C。
实施例2 按照下列步骤制备本发明的富氢保健饮料:
1.交联马铃薯淀粉的制备:取淀粉含量82%以上的马铃薯淀粉100g,加入200mL水调浆后,在常温下超声活化,超声功率为200W,为避免超声时温度升高,采取间歇超声形式,即每隔15min超声10min,总计时间100min。超声活化后,用1mol/L NaOH溶液调节至pH10.0,将其置于37℃水浴锅中,缓慢少量多次加入一氯乙酸钠,即每15min加入0.4g的一氯乙酸钠,中间间隔5min,分四次加完,一氯乙酸钠的总用量为1.6g,期间用电动搅拌器不断搅拌使淀粉发生交联,反应结束后,经盐酸中和至pH 7.0,蒸馏水洗涤三次,4000r/min离心20min,沉淀置于真空度≥0.09MPa,50℃真空干燥箱干燥8h,粉碎过60目筛,得交联马铃薯淀粉;
2.马铃薯皮渣黄酮的制备:将皮层厚度为0.15-0.5mm的马铃薯皮置于不锈钢托盘中铺平,放入50℃真空干燥箱中,真空干燥5h后,以万能粉碎机粉碎过60目筛备用。取粉碎后的马铃薯皮渣100g,加入55%的乙醇溶液1000mL,100MPa高压下浸提20min后,将压力提升至200MPa,10min后再提升至300MPa,超高压提取总时间40min,3500r/min离心20min后,将沉淀物加100mL55%的乙醇溶液,于超声功率为200W的环境下复提20min,合并两次滤液,减压浓缩得马铃薯皮渣黄酮粗提液。100mL粗提液与2g大孔吸附树脂AB-8混合后摇床中振荡吸附24h,滤去未吸附溶液,加入70%乙醇溶液50mL继续于摇床振荡洗脱6h,离心过滤得滤液,减压浓缩后置超低温冰箱-70℃冷冻12h,再由真空冷冻干燥机干燥10h得马铃薯皮渣黄酮;
3.玉米须酚酸的制备:将玉米须低温长时烘干后,取粉碎后的玉米须50g,与50mL90%的乙醇夹带剂一并装入二氧化碳超临界浸提反应釜中,并将釜置于超声功率200W,超声温度60℃的超声清洗设备中,开启二氧化碳进气阀与排气阀,设置釜内压力250bar,出口阀温度100℃,排气1min后关闭排气阀,待超声反应容器与浸提反应釜温度平衡后,开启超声,二氧化碳静态联合超声浸提15min后关闭超声;然后进行二氧化碳动态超临界萃取,二氧化碳流量为2.5L/h,萃取时间为25min,将上述静态动态萃取模式往复3次,得玉米须酚酸提取液。将得到的玉米须酚酸提取液通过大孔吸附树脂XDA-1进行纯化,用60%乙醇溶液以2BV/h的流速进行洗脱,并于327nm处进行峰值检测,以自动组份收集仪收集出峰时间段对应的洗脱溶液,并减压浓缩,超低温冰箱-70℃冷冻12h,真空冷冻干燥10h得玉米须酚酸成品;
4.玉米芯低聚木糖的制备:玉米芯50g与0.3mol/L NaOH溶液1250mL混合,在微波功率为600W,间歇式封闭微波辅助处理10min后,60℃水浴热提30min,3500r/min 条件下离心30min取上清液,用0.1mol/L盐酸中和后,取液体500mL,加1500mL95%乙醇沉淀;再于3500r/min条件下离心30min取沉淀,经氮气吹干得木聚糖粗品。将木聚糖粗品10g加入200mLpH5.0的柠檬酸缓冲液,添加0.1g木聚糖酶(3,0000 U/g)于蒸煮袋中密封。将其放入超高压设备中,设置反应温度50℃,反应压力200MP,反应时间10min后,将温度提升至60℃,反应压力升至300MP,继续反应20min后取出沸水浴灭酶10min,再于3500r/min条件下离心20min得低聚木糖溶液。超低温冰箱-80℃冷冻12h,真空冷冻干燥10h得低聚木糖干粉。将冻干的低聚木糖干粉经超微粉碎设备进行粉碎细化,使其粒度范围D50<1 μm;
5.蒲公英根部含水乙醚提取物的制备:将6-7月份采撷的蒲公英全草摘除叶片部分,45°角斜切斩断至1-2mm厚的根片,至瓦片上于电炉文火焙干,并以万能粉碎机粉碎。取粉碎后的蒲公英根10g,加入2%饱和的含水乙醚150mL,采用索氏提取的回流装置,于35℃浸提回流4h,回收多余的乙醚,得初提液,经氮吹仪,控制分压表于0.3-0.4MPa,氮吹直至膏状变干,吹走残留乙醚。取5g沉淀,分别以95%乙醇20mL、15mL以及10mL溶解、洗涤上述膏状物,再次减压浓缩至膏状,反复操作三次。将膏状物置超低温冰箱-80℃冷冻24 h,再由真空冷冻干燥机冷冻干燥10 h得配方原料;
6.冬虫夏草活性多肽的制备:取野生冬虫夏草干制品,适量喷淋纯净水,使其吸水润涨,并置于-76℃超低温冰箱急速冻结后,于冷冻粉碎机粉碎。取粉碎后的样品10g加入100mL 0.02 mol/L pH 7.5的磷酸盐缓冲液,置于微波-紫外-超声三位一体浸提设备中,微波输出功率360W,输出形式每间隔60s微波加热一次,同时超声工作频率26KHz,输出功率180W提取15min后,超声工作频率变为27KHz,输出功率180W再提取15min后,工作频率28KHz,输出功率不变,再提取15min,完成变频提取。将上述提取液置于真空冷冻干燥设备冷井-70℃,8h完成冻结后,开启真空程序,进行冷冻浓缩,至蛋白含量为5.0%时,完成浓缩程序。取上述5.0%的蛋白溶液20mL,加入0.05g的胰蛋白复合酶(酶活4000 U/g)充分混合后,装入聚乙烯塑料中,置于超高静压反应釜中,设置温度50℃,于超高压200MPa条件下酶解反应4h。将上述超高压联动酶解液于3500r/min离心10min取上清液,接入切向流超滤膜过滤系统,选用4000Da范围内分子膜对其过滤,从而获得特定区段的功能性虫草肽蛋白液。将蛋白液置超低温冰箱-80℃冷冻24h,再由真空冷冻干燥机冷冻干燥10h得配方原料;
7.藏红花乙醇提取物制备:取藏红花干制品5g,加入0.06g复合酶(含纤维素酶(10, 000 U/g)、半纤维素酶(10, 000 U/g)、β-葡萄糖苷酶(5, 000U/g)),再加入50%的乙醇7.5 mL,将其与物料调制成粘稠状,以尽可能快的方式转移至超临界萃取釜中,设定压力300bar,反应温度50℃、静压酶解时间4h,结束后,打开排气阀,设置二氧化碳流量1.5L/h进行动态超临界酶解萃取2h,获得提取液。将提取液至旋转蒸发仪上减压浓缩至膏状。将膏状提取物置于真空冷冻干燥设备冷井-79℃,10h完后冻结,开启真空程序,进行真空冷冻干燥10h,获得配方原料;
8.氢气的制备:以满足色谱仪的高纯氢气发生器为气体源,每分钟最大流量300mL,获得配方原料;
9.将所得马铃薯皮渣黄酮0.8g、玉米须酚酸0.5g、玉米芯低聚木糖2.0g、蒲公英根部含水乙醚提取物0.5g、冬虫夏草活性多肽0.1g以及藏红花乙醇提取物0.1g,加入100mL纯净水,配置成天然饮料原浆后,加入0.4g交联马铃薯淀粉制备天然抑菌淀粉乳溶液,于4℃低温水浴,振荡器转速100r/min条件下震荡3h。将上述经震荡混合后的天然饮料原浆溶液经85℃水浴糊化并不断搅拌,30min后停止搅拌保温孵化30min,再低速搅拌缓慢降至室温,以实现缓慢溶合。将上述溶合好的基料,以德国IKA T18内剪切均浆机以4000 rpm低速均质法处理获得匀浆液;
10.将得到的匀浆液经水力喷射泵的文丘里结构,使其与0.6mL的氢气充分混合接触,氢气源流量设置为60mL/min,完全依靠文丘里气水混合结构,充分自然交溶,实现富氢功能保健饮料成品。多余氢气自然排出并引入大气,最终制备成富氢保健饮料成品。
所述水力喷射泵包括:泵体及泵体上设置的进气口A、饮料浆液进口B和成品饮料出口C。
Claims (1)
1.一种抗菌、强心护肝富氢低糖保健饮料,其特征在于:每100mL纯净水中添加下述重量配比的原料:
经交联马铃薯淀粉:0.2~0.4g
马铃薯皮渣黄酮:0.5~0.8g
玉米须酚酸:0.2~0.5g
玉米芯低聚木糖:0.5~2.0g
蒲公英根部含水乙醚提取物:0.1~0.5g
冬虫夏草活性多肽:0.05~0.1g
藏红花乙醇提取物:0.05~0.1g
氢气:0.50~0.60mL
其制备方法包括如下步骤:
(一)、制备交联马铃薯淀粉
取淀粉含量82%以上的马铃薯淀粉以1:2 g:mL加水调浆后,在超声强度为180-200W,超声温度25℃条件下超声活化100min后,用1mol/L NaOH溶液调节至pH10.0,并将其置于37℃水浴锅中,缓慢少量多次加入一氯乙酸钠,即每15min加入用量为0.3%-0.4%的一氯乙酸钠,中间间隔5min,分四次加完,一氯乙酸钠的总用量为1.2%-1.6%,用电动搅拌器不断搅拌使淀粉发生交联,反应结束后,经盐酸中和至pH 6-7,蒸馏水洗涤三次,4000r/min离心20min,沉淀置于真空度≥0.09MPa,50℃真空干燥箱干燥8h,粉碎过60目筛,得交联马铃薯淀粉;
(二)、制备马铃薯皮渣黄酮
将皮层厚度为0.15-0.5mm的马铃薯皮置于不锈钢托盘中铺平,放入50℃真空干燥箱中,真空干燥5h后,以万能粉碎机粉碎过60目筛备用;采用超高压梯度升压技术,按料液比1:10 g:mL加入45%-55%的乙醇溶液,100MPa高压下浸提10-20min后,将压力提升至200MPa,5-10min后再提升至300MPa,超高压提取总时间20-40min,3500r/min离心20min后,沉淀以1:5 g:mL加入45% 的乙醇溶液采用超声联合两步醇提技术,于超声功率为150-200W,超声温度为25℃条件下复提20min,合并两次滤液,减压浓缩后,得到的马铃薯皮黄酮粗提液与大孔吸附树脂AB-8以50:1 mL:g混合后摇床中振荡吸附24h,滤去未吸附溶液,再以1:25 g:mL加入70%乙醇溶液继续于摇床振荡洗脱4-6h,离心过滤得滤液,减压浓缩后置超低温冰箱-70~-80℃冷冻12h,再由真空冷冻干燥机冷冻干燥10h得马铃薯皮渣黄酮;
(三)、玉米须酚酸的制备
取玉米须低温长时烘干后,将粉碎好的玉米须按1:1 g:mL加入70%-90%乙醇夹带剂,将其再装入二氧化碳超临界浸提反应釜中,置于超声功率180-200W,超声温度50-60℃的超声清洗设备之中,开启二氧化碳进气阀与排气阀,设置反应压力250bar,出口阀温度100℃,排气1min后关闭排气阀,待超声反应容器与浸提反应釜温度平衡后,开启超声,二氧化碳静态联合超声浸提10-15min后关闭超声功率;然后进行动态萃取,二氧化碳流量2.5L/h,萃取时间15-25min,将上述静态动态萃取模式往复3次,得玉米须酚酸提取液;将得到的提取液采用动态吸附洗脱方式进行纯化,取一定量大孔吸附树脂XDA-1装柱,将玉米须酚酸提取液上样后,用60%乙醇溶液以2BV/h的流速进行洗脱,并于327nm处进行峰值检测,以自动组份收集仪收集出峰时间段对应的洗脱溶液,并减压浓缩,低温冰箱-70~-80℃冷冻12h,真空冷冻干燥10h得玉米须酚酸成品;
(四)、制备玉米芯低聚木糖
玉米芯与0.3mol/L的NaOH溶液按料液比1:25 g:mL混合,在微波功率为480-600W,间歇式封闭微波辅助处理8-10min后,60℃水浴热提30min,3500r/min 条件下离心30min取上清液用0.1mol/L盐酸中和,加入3倍体积95%的乙醇沉淀;再于3500r/min条件下离心30min取沉淀,经氮气吹干得木聚糖粗品,将木聚糖粗品用pH5.0的柠檬酸缓冲液配置成4.0%-5.0%的溶液,添加底物1.0%酶活力3,0000 U/g的木聚糖酶于蒸煮袋中密封;将其放入超高压设备中,设置反应温度50℃,反应压力200MP,反应时间5-10min后,将温度提升至60℃,反应压力升至300MP,继续反应15-20min后取出沸水浴灭酶10min,再于3500r/min条件下离心20min得低聚木糖溶液;低温冰箱-70~-80℃冷冻12h,真空冷冻干燥10h得低聚木糖干粉,将冻干的低聚木糖干粉经超微粉碎设备进行粉碎细化,使其粒度范围D50<1μm;
(五)、蒲公英根部含水乙醚提取物的制备
将6-7月份采撷的蒲公英全草摘除叶片部分,45°角斜切斩断至1-2mm厚的根片,至瓦片上于电炉文火焙干,并以万能粉碎机粉碎过60目筛备用;以1:10 g:mL加入2%饱和的含水乙醚为提取剂,采用索氏提取的回流装置,于35℃浸提回流3-4h,回收多余的乙醚,得初提液,经氮吹仪,控制分压表于0.3-0.4MPa,氮吹直至膏状变干,吹走残留乙醚;再分别以1:4,1:3和1:2的比例加入95%乙醇溶解、洗涤上述膏状物,并再次减压浓缩至膏状,反复操作三次,将膏状物置超低温冰箱-70~-80℃冷冻24 h,再由真空冷冻干燥机冷冻干燥10 h得配方原料;
(六)、冬虫夏草活性多肽的制备
取野生冬虫夏草干制品,适量喷淋纯净水,使其吸水润涨,并置于-76℃超低温冰箱急速冻结后,于冷冻粉碎机粉碎过60目筛备用;将粉碎后的样品以1:10 g:mL加入0.02M、pH7.5的磷酸盐缓冲溶液为提取剂,置于微波-紫外-超声三位一体浸提设备中,微波输出功率360W,输出形式每间隔60s微波加热一次,同时超声工作频率26KHz,输出功率180W提取10-15min后,超声工作频率变为27KHz,输出功率180W再提取10-15min后,工作频率28KHz,输出功率不变,再提取10-15min,完成变频提取,将上述提取液置于真空冷冻干燥设备冷井-70~-80℃,8-10 h完后冻结后,开启真空程序,进行冷冻浓缩,至蛋白含量为5.0%时,完成浓缩程序;将上述5.0%的蛋白溶液中加入3%-5%酶活力4000U/g的胰蛋白复合酶充分混合后,装入聚乙烯塑料中,置于超高静压反应釜中,设置温度50℃,于超高压200MPa条件下酶解反应3-4h,将上述超高压联动酶解液于3500r/min离心10min取上清液,接入切向流超滤膜过滤系统,选用4000Da范围内分子膜对其过滤,从而获得特定区段的功能性虫草肽蛋白液,将蛋白液置超低温冰箱-70~-80℃冷冻24h,再由真空冷冻干燥机冷冻干燥10h得配方原料;
(七)、制备藏红花乙醇提取物
取藏红花干制品,加入0.8%-1.2%的复合酶,含酶活力10, 000 U/g的纤维素酶、酶活力10, 000 U/g的半纤维素酶、酶活力5, 000U/g的β-葡萄糖苷酶,按照料液比1:1.5 g:mL加入50%的乙醇溶液,将其与物料调制成粘稠状,以尽可能快的方式转移至超临界萃取釜中,设定超临界反应釜反应压力300 bar,反应温度50℃、静压酶解时间3-4 h,实现静态酶解提取阶段;结束后,打开排气阀,设置二氧化碳流量1.5 L/h进行动态超临界酶解萃取1-2 h,实现动态酶解提取阶段,获得提取液;将提取液至旋转蒸发仪上减压浓缩至膏状,将膏状提取物置于真空冷冻干燥设备冷井-70-80℃,8-10h完后冻结后,开启真空程序,进行真空冷冻干燥10h,以获得配方原料;
(八)、制备氢气
以满足色谱仪的高纯氢气发生器为气体源,每分钟最大流量300mL,并可制得配方原料;
(九)、按照配方比例,合并马铃薯皮渣黄酮、玉米须酚酸、玉米芯低聚木糖、蒲公英根部含水乙醚提取物、冬虫夏草活性多肽以及藏红花乙醇提取物,且以纯净水配置成天然饮料原浆后,加入交联马铃薯淀粉制备天然抑菌淀粉乳溶液,于0-4℃低温水浴,振荡器转速100r/min条件下震荡2-3h,将上述经震荡混合后的天然饮料原浆溶液经85℃水浴糊化并不断搅拌,30-40min后停止搅拌保温孵化20-30 min,再低速搅拌条件下缓慢降至室温,以实现缓慢溶合,将上述溶合好的基料,以德国IKA T18内剪切均浆机以3500-4000rpm低速均质法处理获得匀浆液;
(十)、将上述匀浆液冷却后经水力喷射泵的文丘里结构,使其与0.50~0.60mL氢气充分混合接触,具体操作为:将氢气源流量设置为<60 mL/min,完全依靠文丘里气水混合结构,充分自然交溶,实现富氢功能保健饮料成品,多余氢气自然排出并引入大气,最终制备成富氢保健饮料成品;所述水力喷射泵包括:泵体及泵体上设置的进气口A、饮料浆液进口B和成品饮料出口C。
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