CN111374247A - 一种接骨木莓浓缩汁及其制备方法 - Google Patents
一种接骨木莓浓缩汁及其制备方法 Download PDFInfo
- Publication number
- CN111374247A CN111374247A CN202010305367.XA CN202010305367A CN111374247A CN 111374247 A CN111374247 A CN 111374247A CN 202010305367 A CN202010305367 A CN 202010305367A CN 111374247 A CN111374247 A CN 111374247A
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- Prior art keywords
- elderberry
- liquid
- resin
- concentrated juice
- membrane
- Prior art date
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- Granted
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Classifications
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- A—HUMAN NECESSITIES
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Abstract
一种接骨木莓浓缩汁及其制备方法。本发明制备方法以接骨木莓为原料,经内源酶解、热渗与压榨提取、陶瓷膜澄清、脱苦、提高色值和稳定性、去重金属、膜浓缩等步骤制备接骨木莓浓缩汁。本发明的接骨木莓浓缩汁是一种纯天然、无添加、脱毒、去除苦味、颜色纯正且稳定、去除重金属、无浑浊和后沉淀,具有抗病毒和免疫调节作用的高品质接骨木莓浓缩汁。本发明制备方法通过内源酶解、树脂与纳滤联用去除氰苷等毒性苷和苦味物质以脱除毒性,热渗与压榨实现高效提取,陶瓷膜微滤去除浑浊和后沉淀,专用树脂与超滤联用提高色值和稳定性,螯合树脂去除重金属、反渗透膜与薄膜浓缩联用实现高效浓缩。所述制备方法操作简便,生产成本低,适合工业化生产。
Description
技术领域
本发明涉及植物提取分离技术领域,具体涉及一种接骨木莓浓缩汁及其制备方法。
背景技术
接骨木(Sambucus williamsii Hance)指忍冬科接骨木属(Sambucus L.)植物,主要包括中国接骨木、金叶接骨木、淡黑接骨木、西洋接骨木、加拿大接骨木,其果实即为接骨木,一般呈红色,极少呈蓝紫黑色。
接骨木广泛种植于欧洲、北非、中西亚,它的药用部位有叶、果、花,生于海拔540-1600米的山坡、灌丛、沟边、路旁、宅边等地,在我国产于黑龙江、吉林、辽宁、河北、山西、陕西、山东、安徽、浙江、河南、湖北、广东等省区。
接骨木莓含有丰富的生物活性成分和营养成分,其中,最主要的生物活性成分是多酚类化合物和氰苷;营养成分及其他成分主要是维生素、矿物质、氨基酸等,可鉴别的物质包括维生素A、维生素C、铁和磷。
接骨木莓的多酚类化合物包括花青素类和黄酮类,以及其他高抗氧化物质。花青素是接骨木莓及其他一些水果蔬菜红色、紫色和紫罗兰色的主要原因,也是自然界中广泛存在的一种天然色素;黄酮类化合物,是一种很好的抗氧化剂,能够清除自由基。
氰苷主要存在于接骨木莓的种子中,包括野黑樱苷、黑接骨木苷和吉莉苷等。
此外,接骨木莓尚含有一种血细胞凝集素蛋白-接骨木凝集素Ⅲ(SNA-Ⅲ),对低聚糖表现出很高的亲和力;还含有荚迷酸、α-亚麻酸等不饱合脂肪酸;另含少量甾醇类。
接骨木莓 (Elderberry) 具有“天然医药箱”之称,在欧洲被做为草药和保健食材已有悠久的历史,具有消炎、抗病毒的作用,能抑制流感病毒及舒缓感冒症状,可以用于治疗流感及其引发的咽喉肿痛,咳嗽等上呼吸道感染症状,以及伤风感冒,喝一杯接骨木莓就可以很好的舒缓鼻塞、改善咳嗽症状,效果显著;对心血管保健及增进运动表现也具有相当的潜力,接骨木莓萃取物能显着提升内皮细胞之一氧化氮合成酶 (Endothelial NitricOxide Synthase, eNOS) 的活性;还可提升肌肤防御力和免疫力;接骨木莓含有丰富的不饱和脂肪酸,具有很强的缩水保湿的效果。
现代药理研究发现,接骨木莓具有抗病毒、调节免疫、抗氧化、降血脂、抗肿瘤等作用,临床用于治疗流行性感冒、单纯性疱疹、艾滋病、降血脂、抗氧化应激等。
目前国内外对接骨木莓的研究很多,但相关的专利技术申请较少,且主要围绕提取接骨木果实中的花青素和黄酮为主,但尚无接骨木莓浓缩汁的相关报道。
现有公开以接骨木果实为原料提取的技术内容如下:
CN1052946031A公开了一种从接骨木果实中制备花青素的工业化方法,涉及来源于野生接骨木的花青素的提取、分离方法,本方法先采用高压脉冲电场提取设备对花青素进行提取,再利用膜设备和大孔吸附树脂进行花青素的纯化,得到高纯度的花青素产品。
CN102772468A和CN102807544A公开了一种接骨木果实提取物,采用逆流提取法进行提取得到,所述逆流提取法包括以下步骤:步骤(1),将原料清洗后,低温粉碎;和步骤(2),将粉碎后的原料加入3-6重量/体积倍量、pH值为3-6、质量百分数为10-30%的乙醇水溶液,25-50℃下逆流提取3-6h;以及步骤(3),收集提取液,减压浓缩,即得到所述接骨木果实提取物。
CN101463027A公开了一种接骨木果实中黄酮与花青素的提取和分离方法,包括下述步骤:一、提取:将原料破碎,加入容器中搅拌均匀,浸泡、过滤,得澄清接骨木果实浸出液,备用。二、用大孔树脂吸附柱吸附、洗脱,得浓缩浸膏:三、浸膏干燥,得成品。
以上关于接骨木莓的提取技术均是围绕如何提取接骨木果实中的黄酮和花青素类物质,但现在研究未表明来源于接骨木果实的黄酮和花青素具有抗病毒等作用,这与接骨木莓传统应用于抗病毒及治疗流感有很大的区别,即这些纯化过程去除了接骨木莓的大量生物活性成分,仅得到黄酮和花青素,从而失去原有的多种疗效;且由于接骨木果实中的黄酮和花青素含量较低,市场上又有不同植物来源的黄酮和花青素类产品可替代,实际上来源于接骨木果实的黄酮和花青素在市场上没有竞争力,目前未有企业批量生产和销售该产品。
发明内容
本发明所要解决的技术问题是,克服以上不足,提供一种接骨木莓浓缩汁的制备方法。本发明方法制备的接骨木莓浓缩汁自接骨木莓中提取了多种生物活性物质和营养物质,且无接骨木莓中的氰苷等毒性苷和苦味物质,并保留了接骨木莓的抗病毒和免疫调节作用。
本发明解决其技术问题所采用的技术方案如下:一种接骨木莓浓缩汁的制备方法,包括以下步骤:
(1)内源酶解:将破碎后的接骨木莓投入发酵罐,加入接骨木莓重量2~4倍重量的纯化水,控制温度40~45℃,保温酶解2~4h,升温至90~95℃,保温2.0~3.0 h,然后降温至50~60℃,得酶解物料;
(2)热渗与压榨提取:将酶解物料输送到保温柱,保温50~60℃,放液,放完料液后,压榨固体物料中的料液,再将固体物料投入保温柱,加入所述固体物料重量2~4倍重量的纯化水,升温至50~60℃,保温,放液、压榨各操作1次,合并料液,得提取液;
(3)陶瓷膜澄清:用陶瓷膜成套设备对提取液进行微滤澄清处理,得澄清透明的陶瓷膜滤液;
(4)脱苦:先将陶瓷膜滤液通入装有脱苦树脂的层析柱,然后用纯化水洗柱,收集进柱流出液和水洗液,得树脂脱苦液;再将树脂脱苦液通过纳滤膜成套设备,收集膜上游液,得脱苦液。
(5)提高色值和稳定性:先将脱苦液通过装有增色专用树脂的层析柱,进完料后再用纯化水洗柱,收集进柱流出液和水洗液,得增色液;再将增色液通过截留分子量为20~50KD的超滤膜成套设备,收集膜透过液,得膜分离液;
(6)去重金属:将膜分离液通过装有螯合树脂的层析柱,进完料后再用纯化水洗柱,收集进柱流出液和水洗液,得去重金属液;
(7)膜浓缩:先用反渗透膜成套设备将去重金属液浓缩至固形物含量20~25%,再用薄膜浓缩进一步减压浓缩至固形物含量65~70%,灭菌,得接骨木莓浓缩汁。
优选地,步骤(1)中,所述酶解是采用原存于鲜接骨木莓中的酶水解接骨木莓中的氰苷等毒性苷和苦味物质。
优选地,步骤(2)中,所述放液是每小时放出料液总体积的15~25%。
优选地,步骤(2)中,所述用压榨固体物料中的料液是指榨至固体物料中含水量≤50%。
优选地,步骤(3)中,所述用陶瓷膜成套设备中陶瓷膜的材质为氧化铝或氧化锆,孔径为0.22μm。
优选地,步骤(4)中,所述脱苦树脂选自凝胶型丙烯酸树脂、大孔型丙烯酸树脂、凝胶型苯乙烯系树脂和大孔型苯乙烯系树脂中的一种或多种;优选地,每1000kg接骨木莓用125~200kg脱苦树脂进行脱苦。经研究发现,当选用上述几种树脂作为脱苦树脂时,柱层析过程中,其只吸附皂苷等中性物质,不吸附黄酮及其苷、花青素及其苷等酚酸性物质的一类树脂。
优选地,步骤(4)中,所述纳滤膜的材质为聚酰胺,截留分子量为150~200Da。
优选地,步骤(5)中,所述增色树脂选自凝胶型丙烯酸树脂、大孔型丙烯酸树脂、凝胶型苯乙烯系树脂和大孔型苯乙烯系树脂;优选的,每1000kg接骨木莓采用100~150kg增色树脂增色。采用增色树脂可吸附去除料液中的干扰色,保持料液颜色纯净统一。
优选地,步骤(6)中,每1000kg接骨木莓采用75~125kg螯合树脂去重金属。
优选地,步骤(7)中,所述薄膜浓缩的浓缩条件为温度60~65℃,真空度-0.085Mpa以上。
一种接骨木莓浓缩汁,由以上制备方法制备,按重量计,其主要包括:4~8份花青素及其苷、5~10份黄酮及其苷、15~30份单糖以及低聚糖、3~6份蛋白质以及氨基酸和30~35份水。
本发明制备方法以接骨木莓为原料,原料中含有以花青素和黄酮为主的多酚,以野黑樱苷、黑接骨木苷和吉莉苷为主的氰苷,接骨木凝集素Ⅲ(SNA-Ⅲ),以荚迷酸、α-亚麻酸等为主的不饱合脂肪酸,以及维生素、矿物质、氨基酸等生物活性成分和营养物质。
接骨木莓中的氰苷具有一定的毒性,经发明人研究发现,在一定温度和时间条件下,接骨木莓内源酶可以将氰苷水解成氢氰酸,再通过一定时间的加热以及特定分子量的纳滤膜分离联用技术可以去除氢氰酸,从而去除接骨木莓中氰苷等毒性苷和苦味物质。
经过进一步的研究发现,在50~60℃,仅采用水进行提取时,就可完全提取接骨木莓中的生物活性性成分和营养物质,尤其是花青素和黄酮类物质亦可被完全提取;在50~60℃进行热渗,并让料液以一定速度通过固体物料层(经酶解去毒后的破碎接骨木莓),可保持最大的浓度梯度,从而得到高浓度提取液,既可以避免有机溶剂的加入,还可以用最少的溶剂量进行高效提取;在第一次热渗后,通过压榨获取固体物料层中的剩余料液,并进一步对压榨后的固体物料进行热渗,仍然保持最大的浓度梯度,使料液再次通过固体物料层,通过2次的热渗提取,可以完全提取出原料中的生物活性成分和营养物质。
在去除氰苷和热渗提取后,提取液较浑浊,影响后期树脂和分离操作,且会引起沉淀和后沉淀现象;提取液仍然存在少量氢氰酸和苦味物质,不仅影响口感,而且还具有一定毒性。发明人选择了采用陶瓷膜的错流过滤、微滤澄清技术,将提取液过滤变成澄清透明的溶液。选择了特定的脱苦树脂与特定截留分子量的纳滤膜分离联用技术,在保留接骨木莓生物活性成分和营养物质的同时,完全去除这些残存的少量氢氰酸和苦味物质。此类型脱苦树脂不吸附多酚等活性成分,收集通过脱苦树脂的流出液和水洗液;由于之前已去除氰苷,此处再利用特定分子量的纳滤膜分离技术分离去除氢氰酸,从而得到脱毒脱苦的提取液。此时的脱毒脱苦的提取液中尚含有一定量的杂色(接骨木莓本身显色主要是其中的花青素和黄酮类),杂色影响到最终产品的色泽,选择特定增色树脂树脂去除杂色,以增强主显色为花青素和黄酮的混合色(即为增色过程);增色后的溶液需要进一步提高稳定性,则采用具有一定截留分子量的超滤膜收集花青素和黄酮的区段,以提高主显色的稳定性。
接骨木原料一般是野生,会存在一定的重金属,影响安全性,需要去除。螯合树脂对存在于料液中的重金属具有捕集作用,而不影响其他成分,因此,将料液通过装有螯合树脂的层析柱,从而去除重金属。然后,采用反渗透膜浓缩至固形物含量30%,在常温下,进行高效浓缩,从而节省浓缩成本;接下来,在减压条件下,将料液浓缩至高固形物含量,从30%以内提高到70%左右,经过杀菌后,得到接骨木莓浓缩汁。
本发明的有益效果在于:
(1)本发明提供了一种接骨木莓浓缩汁,在接骨木产品系列中属于新产品,具有纯天然、无添加、脱毒、去除苦味、颜色纯正且稳定、去除重金属、无浑浊和后沉淀,具有抗病毒和免疫调节作用;其固形物含量65~70%,为红褐色至紫褐色黏稠液体;主要组成:花青素及其苷4~8%、黄酮及其苷5~10%、单糖以及低聚糖15~30%、蛋白质和氨基酸3~6%、其他成分15~25%、水30~35%。
(2)本发明方法仅采用水充分提取了接骨木莓中的生物活性成分和营养物质,保留原汁原味,纯天然,无添加,使产品接骨木莓浓缩汁具有传统意义上的抗病毒和免疫调节作用;去除了浓缩汁中的氰苷等毒性苷和苦味物质,以脱除毒性,提高使用安全性;还去除浓缩汁中的机械杂质和引起浑浊的物质,保持浓缩汁澄清透明,无浑浊和后沉淀;增强了浓缩汁的颜色,使其主显明显的红色或紫色,并提高了颜色的稳定性;还去除了浓缩汁中的重金属,提高安全性;并建立了适合植物提取物工厂使用的、较为简单的生产工艺,能规模生产出优质的接骨木莓浓缩汁工业产品,按照本发明方法所得接骨木莓浓缩汁,每1000kg原料可产100kg以上成品,产品收率>10%。
(3)本发明方法利用原存于接骨木莓中的内源酶水解氰苷等毒性苷和苦味物质;并利用类似渗漉提取的热渗技术,结合果汁压榨技术,实现了对接骨木莓中生物活性物质和营养物质的高效提取;利用特定树脂和特定的纳滤膜分离联用技术去除苦味和毒性物质;利用特定树脂与超滤膜分离技术联用,实现了产品增色;利用特定树脂去除重金属;最终利用反渗透膜浓缩与薄膜浓缩实现高效浓缩,从而制备了高品质产品-接骨木莓浓缩汁。
本发明所述接骨木(Sambucus williamsii Hance)指忍冬科接骨木属(SambucusL.)植物,所述接骨木莓主要包括中国接骨木、金叶接骨木、淡黑接骨木、西洋接骨木、加拿大接骨木的新鲜成熟果实,或鲜果的冷冻储存品。
具体实施方式
以下结合实施例对本发明进行进一步的说明。
本发明实施例所使用的原料接骨木莓为淡黑接骨木的新鲜成熟果实,购于辽宁;所使用纯化水为生产车间用二级纯水设备制备,所使用的化学试剂和原辅材料,如无特殊说明,均通过常规商业途径获得。
本发明实施例中,花青素及其苷、黄酮及其苷等多酚类物质用UV法测定;糖类物质用滴定法测定;蛋白质和氨基酸类根据《中国药典》2015版用凯氏定氮法测定;固形物含量根据《中国药典》2015版用干燥法测定。
实施例1
本实施例包括以下步骤:
(1)内源酶解:将经鲜果破碎机打浆破碎后的新鲜接骨木莓1000kg投入6m3发酵罐,加入2500L纯化水,加热升温至42℃,保温酶解3h,升温至93℃,保温2.3h,灭活内源酶及脱毒,通水冷却,降低温度至56℃,得酶解物料;
(2)热渗与压榨提取:将酶解物料输送到专用的不锈钢保温柱,保温56℃,放液,控制流速为450L/h,使料液逐渐通过固体物料层,放完料液后,用压榨机榨干固体物料中的料液,使固体物料中的含水量为47%,得3050L提取液,430kg固体物料;
再将430kg固体物料投入保温柱,加入1500L纯化水,加热升温至52℃,保温52℃,放液,控制流速为280L/h,使料液逐渐通过固体物料层,放完料液后,用压榨机榨干固体物料中的料液,使固体物料中的含水量为49%,得1550L提取液,372kg固体物料;
合并提取液,通水冷却至室温,得4600L提取液;
(3)陶瓷膜澄清:用材质为氧化锆、孔径0.22μm的陶瓷膜成套设备对提取液进行微滤澄清处理,得澄清透明的陶瓷膜滤液;
(4)脱苦:将陶瓷膜滤液通过装有180kg,已用酸碱处理好的LSA-600树脂(大孔型苯乙烯系树脂)的层析柱,进完料后再用300L纯化水洗柱,收集进柱流出液和水洗液,得4800L树脂脱苦液;
再将树脂脱苦液通过材质为聚酰胺、截留分子量为150Da的纳滤膜成套设备,当上游液体积降至800L时,往其中加入800 L纯化水,继续过膜;后续再降至800L时,同法加水操作2次,收集加水3次后的上游液,得800L脱苦液。
(5)提高色值和稳定性:先将脱苦液加纯化水稀释至2800L,再通过装有120kg,已用酸碱处理好的LSA-900B树脂(大孔型苯乙烯系树脂)的层析柱,进完料后再用200L纯化水洗柱,收集进柱流出液和水洗液,得2950L增色液;
再将增色液通过截留分子量为50KD的超滤膜成套设备,收集膜透过液,得膜分离液。
(6)去重金属:将膜分离液通过装有90kg,已用酸碱处理好的LSC-100树脂的层析柱,进完料后再用150纯化水洗柱,收集进柱流出液和水洗液,得3000L去重金属液。
(7)膜浓缩:先用反渗透膜成套设备将去重金属液浓缩至固形物含量24%,再用薄膜浓缩进一步减压浓缩(温度62℃,真空度-0.085Mpa)至固形物含量66.2%,得114kg浓缩液,灭菌,得接骨木莓浓缩汁。
根据需求将接骨木莓浓缩汁进行包装,得接骨木莓浓缩汁。
经检测,花青素及其苷6.2%、黄酮及其苷8.4%、单糖以及低聚糖25.6%、蛋白质和氨基酸4.7%、其他成分21.3%、水33.8%。
浓缩汁的固形物含量66.2%。
实施例2
(1)内源酶解:将经鲜果破碎机打浆破碎后的新鲜接骨木莓400kg投入3m3发酵罐,加入1400L纯化水,加热升温至41℃,保温酶解3.5h,升温至92℃,保温2.5h,灭活内源酶及脱毒,通水降温至54℃,得酶解物料;
(2)热渗与压榨提取:将酶解物料输送到不锈钢保温柱,保温54℃,放液,控制流速为350L/h,使料液逐渐通固体物料层,放完料液后,用压榨机榨干固体物料中的料液,使固体物料中的含水量为49%,得1610L提取液,178kg固体物料;
再将178kg固体物料投入保温柱,加入500L纯化水,加热升温至57℃,保温57℃,放液,控制流速为125L/h,使料液逐渐通过固体物料层,放完料后,用压榨机榨干固体物料中的料液,使固体物料中的含水量为46%。得525L提取液,146kg固体物料;
合并提取液,通水冷却至室温,得2135L提取液。
(3)陶瓷膜澄清:用材质为氧化锆、孔径0.22μm的陶瓷膜成套设备对提取液进行微滤澄清处理,得澄清透明的陶瓷膜滤液;
(4)脱苦:将提取液通过装有60kg,已用酸碱处理好的LX-900树脂(大孔型丙烯酸系树脂)的层析柱,进完料再用100L纯化水洗柱,收集进柱流出液和水洗液,得2200L树脂脱苦液;
再将树脂脱苦液通过材质为聚酰胺、截留分子量为180Da的纳滤膜成套设备,当上游液体积降至350L时,往其中加入350 L纯化水,继续过膜;后续再降至350L时,同法加水操作2次,收集加水3次后的上游液,得350L脱苦液。
(5)提高色值和稳定性:先将脱苦液加纯化水稀释至1200L,再通过装有50kg,已用酸碱处理好的LSA-900C(大孔型苯乙烯系树脂)树脂的层析柱,进完料后再用80L纯化水洗柱,收集进柱流出液和水洗液,得1250L增色液;
再将增色液通过截留分子量为30KD的超滤膜成套设备,收集膜透过液,得膜分离液;
(6)去重金属:将膜分离液通过装有40kg,已用酸碱处理好的LSC-100树脂的层析柱,进完料后再用60L纯化水洗柱,收集进柱流出液和水洗液,得1300L去重金属液;
(7)膜浓缩:先用反渗透膜成套设备将去重金属液浓缩至固形物含量22%,再用薄膜浓缩进一步减压浓缩(温度64℃,真空度-0.089Mpa)至固形物含量69.1%,得45.1kg浓缩液,灭菌,得接骨木莓浓缩汁。
根据需求将接骨木莓浓缩汁进行不同规格包装,得到接骨木莓浓缩汁产品。
经检测,花青素及其苷7.1%、黄酮及其苷9.2%、单糖以及低聚糖26.8%、蛋白质和氨基酸5.7%、其他成分21.1%、水30.1%。
浓缩汁的固形物含量69.1%。
对比例 1
其他步骤和实施例1相同,区别在于去除步骤(1)内源酶解,最终得到106kg接骨木莓浓缩汁成品。经口尝比较,实施例1所得接骨木莓浓缩汁成品无明显苦味,入口好,而对比例1所得成品苦味明显,并带涩味,难以入口;经检测,花青素及其苷4.2%、黄酮及其苷5.4%、单糖以及低聚糖28.7%、蛋白质和氨基酸5.6%、其他成分21.5%、水34.6%。
浓缩汁的固形物含量65.4%。
本对比例制备的接骨木莓浓缩汁不仅仅具有明显的苦味,其花青素及其苷、黄酮及其苷的含量也低于实施例1制备的接骨木莓浓缩汁,可见步骤(1)与后续步骤具有协同作用,不仅有利于去除氰苷和苦味物质,还有利于提取花青素及其苷、黄酮及其苷。
对比例 2
其他步骤和实施例2相同,区别在于步骤(2)热渗与压榨提取,所用保温温度为85℃,最终得到42.9kg接骨木莓浓缩汁成品。经检测,花青素及其苷3.1%、黄酮及其苷6.5%、单糖以及低聚糖29.1%、蛋白质和氨基酸6.1%、其他成分21.3%、水33.9%。
浓缩汁的固形物含量66.1%。
相较于实施例2,本对比例的热渗提取步骤的保温温度较高,使得制备的接骨木莓浓缩汁中的花青素及其苷、黄酮及其苷的含量低,由此可见,提高保温温度,不仅不能有利于接骨木莓中物质的提取,还将破坏花青素和黄酮等生物活性成分和营养物质,因此,本发明制备方法的热渗提取保温温度保持在50~60℃,能够完全提取接骨木莓中的生物活性成分和营养物质。
Claims (10)
1.一种接骨木莓浓缩汁的制备方法,其特征在于,包括以下步骤:
(1)内源酶解:将破碎后的接骨木莓投入发酵罐,加入接骨木莓重量2~4倍重量的纯化水,控制温度40~45℃,保温酶解2~4h,升温至90~95℃,保温2.0~3.0 h,然后降温至50~60℃,得酶解物料;
(2)热渗与压榨提取:将酶解物料输送到保温柱,保温50~60℃,放液,放完料液后,压榨固体物料中的料液,再将固体物料投入保温柱,加入所述固体物料重量2~4倍重量的纯化水,升温至50~60℃,保温,放液、压榨各操作1次,合并料液,得提取液;
(3)陶瓷膜澄清:用陶瓷膜成套设备对提取液进行微滤澄清处理,得澄清透明的陶瓷膜滤液;
(4)脱苦:先将陶瓷膜滤液通入装有脱苦树脂的层析柱,然后用纯化水洗柱,收集进柱流出液和水洗液,得树脂脱苦液;再将树脂脱苦液通过纳滤膜成套设备,收集膜上游液,得脱苦液;
(5)提高色值和稳定性:先将脱苦液通过装有增色专用树脂的层析柱,进完料后再用纯化水洗柱,收集进柱流出液和水洗液,得增色液;再将增色液通过截留分子量为20~50KD的超滤膜成套设备,收集膜透过液,得膜分离液;
(6)去重金属:将膜分离液通过装有螯合树脂的层析柱,进完料后再用纯化水洗柱,收集进柱流出液和水洗液,得去重金属液;
(7)膜浓缩:先用反渗透膜成套设备将去重金属液浓缩至固形物含量20~25%,再用薄膜浓缩进一步减压浓缩至固形物含量65~70%,灭菌,得接骨木莓浓缩汁。
2.根据权利要求1所述接骨木莓浓缩汁的制备方法,其特征在于,步骤(1)中,所述酶解是用原存于鲜接骨木莓中的酶水解接骨木莓中的氰苷等毒性苷和苦味物质。
3.根据权利要求1或2所述接骨木莓浓缩汁的制备方法,其特征在于,步骤(2)中,所述放液是每小时放出料液总体积的15~25%;所述压榨固体物料中的料液是指榨至固体物料中含水量≤50%。
4.根据权利要求1-3任一项所述接骨木莓浓缩汁的制备方法,其特征在于,步骤(3)中,所述用陶瓷膜成套设备中陶瓷膜的材质为氧化铝或氧化锆,孔径为0.22μm。
5.根据权利要求1-4任一项所述接骨木莓浓缩汁的制备方法,其特征在于,步骤(4)中,所述脱苦树脂选自凝胶型丙烯酸树脂、大孔型丙烯酸树脂、凝胶型苯乙烯系树脂和大孔型苯乙烯系树脂中的一种或多种;优选地,每1000kg接骨木莓用125~200kg脱苦树脂进行脱苦。
6.根据权利要求1-5任一项所述接骨木莓浓缩汁的制备方法,其特征在于,步骤(4)中,所述纳滤膜的材质为聚酰胺,截留分子量为150~200Da。
7.根据权利要求1-6任一项所述接骨木莓浓缩汁的制备方法,其特征在于,步骤(5)中,所述增色树脂选自凝胶型丙烯酸树脂、大孔型丙烯酸树脂、凝胶型苯乙烯系树脂和大孔型苯乙烯系树脂中的一种或多种;优选的,每1000kg接骨木莓采用100~150kg增色树脂增色。
8.根据权利要求1-7任一项所述接骨木莓浓缩汁的制备方法,其特征在于,步骤(6)中,每1000kg接骨木莓采用75~125kg螯合树脂去重金属。
9.根据权利要求1-8任一项所述接骨木莓浓缩汁的制备方法,其特征在于,步骤(7)中,所述薄膜浓缩的浓缩条件为温度60~65℃,真空度-0.085Mpa以上。
10.一种接骨木莓浓缩汁,其特征在于,所述接骨木莓浓缩汁由权利要求1~9任一项所述制备方法制备按重量计,其主要包括:4~8份花青素及其苷、5~10份黄酮及其苷、15~30份单糖以及低聚糖、3~6份蛋白质以及氨基酸和30~35份水。
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CN112094741A (zh) * | 2020-08-13 | 2020-12-18 | 赣州禾绿康健生物技术有限公司 | 一种接骨木莓提取液的免有机溶剂提纯设备 |
CN112094741B (zh) * | 2020-08-13 | 2021-07-09 | 赣州禾绿康健生物技术有限公司 | 一种接骨木莓提取液的免有机溶剂提纯设备 |
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