CN116584659A - 一种含有硒多肽的产品及其制备方法 - Google Patents

一种含有硒多肽的产品及其制备方法 Download PDF

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CN116584659A
CN116584659A CN202310585680.7A CN202310585680A CN116584659A CN 116584659 A CN116584659 A CN 116584659A CN 202310585680 A CN202310585680 A CN 202310585680A CN 116584659 A CN116584659 A CN 116584659A
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selenium
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cyclodextrin
polypeptide
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李相钊
张中庆
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Shandong Zhishan Selenium Biotechnology Co ltd
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Abstract

本发明公开了一种含有硒多肽的产品,所述含有硒多肽的产品包括如下质量份数的成分:硒多肽、菊粉、植物提取物、食用菌粉、果蔬粉、改良剂、多糖;其中,所述改良剂为环糊精接枝的聚丙烯酸衍生物。通过将中间产物接枝到氨基‑β‑环糊精改善了氨基‑β‑环糊精,可以提高氨基‑β‑环糊精对硒多肽的包结能力,使得粉末的和硒多肽充分混合,改善粉末和硒多肽的相容性、分散性和调和均一性,从而提高了产品压片后,硒多肽在压片中的释放均匀性。

Description

一种含有硒多肽的产品及其制备方法
技术领域
本发明属于多肽技术领域,具体涉及一种含有硒多肽的产品及其制备方法。
背景技术
富硒复合蛋白不仅含有大量的人和动植物所需的蛋白质,还含有微量元素硒等,是微量元素的供给体,在养生保健、清除自由基、抗衰老、抗辐射、抗癌变、提高免疫力等方面,对人体健康具有多种免疫和生物学功能。
硒不仅是人体和动植物必需的微量元素,而且对人体和动物有很多有益功能,利用硒的独特化学和生物化学特性及相关交叉学科的研究,取得了举世瞩目的研究成果。近些年,随着硒及其化合物分子水平研究,对硒蛋白、硒酶和其它硒化合物的生理功能有了新的认识和新的突破,科学研究成果揭示了硒与人类健康密切相关。
申请号为CN200410102984.0中国授权专利公开一种具有消除体内自由基抗氧化保健功能的天然抗氧化果蔬保健食品,该专利所得到的抗氧化营养素有相互补充及协同作用,可以起到清除体内自由基,改善脂代谢、预防高血脂,对中老年人身体保健起到辅助作用。
而目前现有技术中硒多肽的产品在压片之后,在保存过程中会多肽的稳定性较差,在存储时容易变质,影响产品的质量。
因此,亟需找到一种含有硒多肽的产品及其制备方法,来解决上述问题。
发明内容
针对现有技术中,本发明将通过添加聚丙烯酸衍生物的改良剂添加在含有硒多肽的产品内,可以避免保存过程使得硒多肽的稳定性下降,硒多肽的产品在压片之后,在保存过程中会多肽的稳定性较差,在存储时容易变质,影响产品的质量的问题。
本发明公开了一种含有硒多肽的产品,所述含有硒多肽的产品包括如下质量份数的成分:
其中,所述改良剂为环糊精接枝的聚丙烯酸衍生物。
进一步地,所述果蔬粉的原料选自堇叶碎米荠、天瓜粉、西兰花、沙棘果、樱桃李的一种或多种;所述食用菌粉选自平菇、猴头菇、香菇、蛹虫草、灵芝中的一种或多种。
进一步地,所述多糖选自植物多糖或动物多糖。
进一步地,所述植物提取物选自竹叶黄酮、植物甾醇的一种或两种。
本发明还提供了含有硒多肽的产品的制备方法,所述含有硒多肽的产品的制备方法包括如下步骤:
S1、氮气保护下,将表面活性剂、分子量调节剂和pH缓冲剂加入水中,加热,再加入甲基丙烯酸和丙烯酸烷基酯和引发剂,加热反应得到聚丙烯酸衍生物;
S2、再向其中加入NHS和EDCI,并用冰浴冷却,得到中间产物;
S3、向其中加入氨基-β-环糊精,混合反应,得到粗产物;
S4、将所述粗产物透析3-5d,并除水,得到改良剂;
S5、将分别称取的果蔬粉、面粉、植物提取物、改良剂、多糖先后倒入搅拌釜内,加入200-500份的水,并加热到55-60℃,搅拌30-35min,加入硒多肽,继续搅拌25min后,取出凉至恒温;
S6、用研磨器皿将凉到恒温的组合物研磨到150-200目,70℃烘干10-12h,冷却至常温得到含有硒多肽的产品。
进一步地,所述丙烯酸烷基酯中的烷基选自C8-C22的烷基。
进一步地,所述表面活性剂的浓度为含有硒多肽的产品质量份的1-3wt%。
进一步地,所述表面活性剂选自十二烷基硫酸钠、琥珀酸二辛酯磺酸钠、聚山梨醇酯80中的一种或多种;
优选地,所述表面活性剂为十二烷基硫酸钠。
进一步地,所述中间产物与氨基-β-环糊精的质量比为1:10-1:5。
进一步地,步骤S1中,所述反应的时间为10-24h。
进一步地,步骤S1中,所述反应的温度为0-5℃。
进一步地,所述表面活性剂、分子量调节剂、pH缓冲剂、甲基丙烯酸、丙烯酸烷基酯、引发剂的质量比为1.5-2:0.2-0.4:0.1-0.3:8-12:15-25:0.1-0.3。
进一步地,所述聚丙烯酸衍生物、NHS和EDCI的质量比为30-36:29-35:96-103。
进一步地,所述pH缓冲剂选自碳酸氢钠、磷酸二氢钾、柠檬酸钾中的一种或多种。
优选地,所述pH缓冲剂为碳酸氢钠。
进一步地,所述分子量调节剂选自月桂醇。
优选地,所述引发剂选自过硫酸钾。
本发明具有以下有益技术效果:
通过将中间产物接枝到氨基-β-环糊精改善了氨基-β-环糊精,可以提高氨基-β-环糊精对硒多肽的包结能力,使得粉末的和硒多肽充分混合,改善粉末和硒多肽的相容性、分散性和调和均一性,从而提高了产品压片后,硒多肽在压片中的释放均匀性。
具体实施方式
以下结合具体实施例来进一步说明本发明,但实施例并不对本发明做任何形式的限定。除非特别说明,本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
除非特别说明,以下实施例所用试剂和材料均为市购。
所述硒多肽采购自江苏中农科食品工程有限公司。
所述菊粉采购自上海陶术生物科技有限公司。
所述食用菌粉为香菇粉,采购自浙江天和食品有限公司。
所述果蔬粉为天瓜粉,采购自上海源叶生物科技有限公司牌号为B26236的天瓜粉。
所述十二烷基硫酸钠采购自上海麦克林生化科技股份有限公司牌号为S885172的十二烷基硫酸钠。
所述月桂醇采购自上海阿拉丁生化科技股份有限公司牌号为D112297的月桂醇。
所述碳酸氢钠采购自上海迈瑞尔生化科技有限公司牌号为M88765的碳酸氢钠。
所述甲基丙烯酸采购自上海迈瑞尔生化科技有限公司牌号为M26917的甲基丙烯酸。
所述丙烯酸二十二烷酯采购自武汉荣灿生物科技有限公司牌号为RC01913的丙烯酸二十二烷酯。
所述过硫酸钾采购自山东省冶金科学研究院有限公司牌号为SJ201168的过硫酸钾。
所述NHS采购自上海阿拉丁生化科技股份有限公司牌号为H109330的NHS。
所述EDCI采购自上海麦克林生化科技股份有限公司牌号为N823219的EDCI。
所述氨基-β-环糊精采购自北京华威锐科化工有限公司牌号为HWG45656的氨基-β-环糊精。
实施例1
一种含有硒多肽的产品,所述含有硒多肽的产品包括如下质量份数的成分:
其中,所述改良剂为环糊精接枝的聚丙烯酸衍生物。
本发明还提供了含有硒多肽的产品的制备方法,所述含有硒多肽的产品的制备方法包括如下步骤:
S1、氮气保护下,将所述十二烷基硫酸钠、月桂醇和碳酸氢钠加入水中,使pH为6,加热75℃,再滴加甲基丙烯酸和丙烯酸二十二烷酯和过硫酸钾,滴加2h,滴加完成后保温反应2h,得到聚丙烯酸衍生物;其中,所述十二烷基硫酸钠、月桂醇、碳酸氢钠、甲基丙烯酸、丙烯酸二十二烷酯、过硫酸钾的质量比为1.5:0.2:0.1:8:15:0.1。
S2、再向其中加入NHS和EDCI,并用冰浴冷却10min,得到中间产物;其中,所述聚丙烯酸衍生物、NHS和EDCI的质量比为30:29:96;
S3、向其中加入氨基-β-环糊精,混合在0℃反应10h,得到粗产物;其中,所述中间产物与氨基-β-环糊精的质量比为1:10;
S4、将所述粗产物透析3d,并除水,得到改良剂;
S5、将分别称取上述质量份数的天瓜粉、菊粉、竹叶黄酮、香菇粉、改良剂、可溶性大豆多糖先后倒入搅拌釜内,加入200份的水,并加热到55℃,搅拌30min,加入硒多肽,继续搅拌25min后,取出凉至恒温;
S6、用研磨器皿将凉到恒温的组合物研磨到150目,70℃烘干10h,冷却至常温得到含有硒多肽的产品。
实施例2
一种含有硒多肽的产品,所述含有硒多肽的产品包括如下质量份数的成分:
其中,所述改良剂为环糊精接枝的聚丙烯酸衍生物。
本发明还提供了含有硒多肽的产品的制备方法,所述含有硒多肽的产品的制备方法包括如下步骤:
S1、氮气保护下,将十二烷基硫酸钠、月桂醇和碳酸氢钠加入水中,使pH为6,加热78℃,再滴加甲基丙烯酸和丙烯酸二十二烷酯和过硫酸钾,滴加2h,滴加完成后保温反应2h,得到聚丙烯酸衍生物;其中,所述十二烷基硫酸钠、月桂醇、碳酸氢钠、甲基丙烯酸、丙烯酸二十二烷酯、过硫酸钾的质量比为1.7:0.3:0.2:10:20:0.2;
S2、再向其中加入NHS和EDCI,并用冰浴冷却10min,得到中间产物;其中,所述聚丙烯酸衍生物、NHS和EDCI的质量比为33:32:100;
S3、向其中加入氨基-β-环糊精,混合在2℃反应17h,得到粗产物;其中,所述中间产物与氨基-β-环糊精的质量比为1:10;
S4、将所述粗产物透析4d,并除水,得到改良剂;
S5、将分别称取上述质量份数的天瓜粉、菊粉、竹叶黄酮、香菇粉、改良剂、可溶性大豆多糖先后倒入搅拌釜内,加入350份的水,并加热到57℃,搅拌33min,加入硒多肽,继续搅拌25min后,取出凉至恒温;
S6、用研磨器皿将凉到恒温的组合物研磨到180目,70℃烘干11h,冷却至常温得到含有硒多肽的产品。
实施例3
一种含有硒多肽的产品,所述含有硒多肽的产品包括如下质量份数的成分:
其中,所述改良剂为环糊精接枝的聚丙烯酸衍生物。
本发明还提供了含有硒多肽的产品的制备方法,所述含有硒多肽的产品的制备方法包括如下步骤:
S1、氮气保护下,将月桂醇、十二烷基硫酸钠和碳酸氢钠加入水中,使pH为6,加热80℃,再滴加甲基丙烯酸、丙烯酸二十二烷酯和过硫酸钾,滴加2h,滴加完成后保温反应2h,得到聚丙烯酸衍生物;其中,所述十二烷基硫酸钠、月桂醇、碳酸氢钠、甲基丙烯酸、丙烯酸二十二烷酯、过硫酸钾的质量比为2:0.4:0.3:12:25:0.3;
S2、再向其中加入NHS和EDCI,并用冰浴冷却10min,得到中间产物;其中,所述聚丙烯酸衍生物、NHS和EDCI的质量比为36:35:103;
S3、向其中加入氨基-β-环糊精,混合在5℃反应24h,得到粗产物;其中,所述中间产物与氨基-β-环糊精的质量比为1:10;
S4、将所述粗产物透析5d,并除水,得到改良剂;
S5、将分别称取上述质量份数的天瓜粉、菊粉、竹叶黄酮、香菇粉、改良剂、可溶性大豆多糖先后倒入搅拌釜内,加入500份的水,并加热到60℃,搅拌35min,加入硒多肽,继续搅拌25min后,取出凉至恒温;
S6、用研磨器皿将凉到恒温的组合物研磨到200目,70℃烘干12h,冷却至常温得到含有硒多肽的产品。
对比例1
对比例1与实施例1所述的一种含有硒多肽的产品的制备方法、所用原料均相同,唯一不同在于,所述改良剂采用的是没有改性的聚丙烯酸和氨基-β-环糊精反应得到。
所述聚丙烯酸采购自上海麦克林生化科技有限公司牌号为P822497的聚丙烯酸。
测试例
为了测定缓释性,我们将样品中的硒多肽预先和1wt%的色素胭脂红共混均匀,然后再进一步制得实施例1和对比例1中的产品,经压片机压片为口服的药片状的片剂。
测试方法1:将上述片剂分别投入200ml的去离子水中,观察色素溢出的速率和均匀性,并用文字描述。
测试方法2:另外,召集研发中心志愿者20名,将上述实施例1和对比例1中的产品(不添加色素)的片剂口服,记录口感,并用文字描述。
表1:实施例1和对比例1中相关数据比较
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。

Claims (10)

1.一种含有硒多肽的产品,其特征在于,所述含有硒多肽的产品包括如下质量份数的成分:
其中,所述改良剂为环糊精接枝的聚丙烯酸衍生物。
2.根据权利要求1所述含有硒多肽的产品,其特征在于,所述果蔬粉的原料选自堇叶碎米荠、天瓜粉、西兰花、沙棘果、樱桃李的一种或多种;所述食用菌粉选自平菇、猴头菇、香菇、蛹虫草、灵芝中的一种或多种。
3.根据权利要求1所述含有硒多肽的产品,其特征在于,所述多糖选自植物多糖或动物多糖。
4.根据权利要求1所述含有硒多肽的产品,其特征在于,所述植物提取物选自竹叶黄酮、植物甾醇的一种或两种。
5.如权利要求1-4任一项所述含有硒多肽的产品的制备方法,其特征在于,所述含有硒多肽的产品的制备方法包括如下步骤:
S1、氮气保护下,将表面活性剂、分子量调节剂和pH缓冲剂加入水中,加热,再加入甲基丙烯酸和丙烯酸烷基酯和引发剂,加热反应,得到聚丙烯酸衍生物;
S2、再向其中加入NHS和EDCI,并用冰浴冷却,得到中间产物;
S3、向其中加入氨基-β-环糊精,混合反应,得到粗产物;
S4、将所述粗产物透析3-5d,并除水,得到改良剂。
6.根据权利要求5所述含有硒多肽的产品的制备方法,其特征在于,所述表面活性剂的浓度为溶液的1-3wt%。
7.根据权利要求5所述含有硒多肽的产品的制备方法,其特征在于,所述中间产物与氨基-β-环糊精的质量比为1:10-1:5。
8.根据权利要求5所述含有硒多肽的产品的制备方法,其特征在于,步骤S1中,所述反应的时间为10-24h。
9.根据权利要求5所述含有硒多肽的产品的制备方法,其特征在于,步骤S2中,所述反应的温度为0-5℃。
10.根据权利要求5所述含有硒多肽的产品的制备方法,其特征在于,所述甲基丙烯酸和丙烯酸烷基酯的摩尔比为1-1.5:1-2。
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