CN101747222A - 甘氨酸螯合牡蛎钙水相合成方法及高钙酱油的制备 - Google Patents
甘氨酸螯合牡蛎钙水相合成方法及高钙酱油的制备 Download PDFInfo
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Abstract
一种甘氨酸螯合牡蛎钙水相制备方法及高钙酱油的制备，本发明选用生物钙源---牡蛎壳充分灰化后的灰分为主要原料，与甘氨酸在水相条件下控制温度在90～100℃范围内制备甘氨酸螯合牡蛎钙，以投入灰分与甘氨酸的质量比，反应时间及加水量为三个影响因素，通过优化反应条件，得出螯合效果最佳且经济实用的方法。因氨基酸螯合物便于人体吸收，故将所制备的甘氨酸螯合牡蛎钙按一定比例投放到酱油中，强化营养。
Description
技术领域
本发明涉及一种利用生物钙源---牡蛎壳制备甘氨酸螯合钙的方法及高钙酱油制备，属食品科学技术领域。
背景技术
钙是人们熟知的一种无机质营养素，是继C、H、N、O在人体中第5位构成元素。它同人体的神经传导、心膊调节、肌肉收缩、血液凝固、酶激活、内分泌调节等密切相关，对人体生长发育和健康维持起着极为重要的作用。到目前为止，钙制剂的发展历经了无机钙盐、传统的简单的有机钙盐以及新型可溶性有机钙三代，其中前两代均不易人体吸收，吸收利用率差，因此开发安全高效的钙制剂---氨基酸螯合钙，成为研究热点。
在现有的氨基酸螯合钙的研究技术中，公开号为CN 101220383A，申请号为200810025894.4的专利“一种制备氨基酸钙的方法”，其工艺是将鱼骨酶解得到蛋白源，采用嗜酸乳杆菌和嗜热乳酸链球菌发酵使鱼骨中的钙游离出来，与酶解蛋白液中的氨基酸结合生成离子态的氨基酸钙，其工艺程序复杂，需要先酶解得到氮源，再发酵得到钙源，产量少，不适合大批量生产。公开号为CN 101225050A，申请号为200810059641.9的专利“一种甘氨酸钙的制备方法”，其工艺是甘氨酸与固碱反应生成甘氨酸钠盐，然后加入氯化钙，调pH值，加热搅拌至浓缩结晶，真空干燥得[Ca(C2H5NO2)2Cl2]，其工艺中主要以无机药品合成，且产物为离子形式，产物纯度不高。
牡蛎壳矿物质以钙元素为主，钙含量为39.78％±0.23％，另有锌、钡、铜、铁、镁、锰、铬、锶等多种人体所需微量无机元素，其保健价值可于龙骨相媲美，具有很高的药用保健价值。将牡蛎壳高温煅烧制备活性钙的技术已经得到广泛应用，高温煅烧有利于牡蛎壳中其他金属气化，如铬、汞等，还有助于部分金属如Zn、Pb转变为易挥发的化合物而挥发，减少杂质金属的同时除去有害重金属，得到高含量的钙粉。本专利采用纯天然生物钙源---牡蛎壳，既合理利用钙剂资源，变废为宝，又能提高产品的安全性，是一种优良的原料。而据大量研究表明，钙与氨基酸结合后，进入细胞之前，必须首先通过小肠细胞壁上的钙通道，而钙通道对分子大小有严格要求，分子量越小越容易通过，而甘氨酸是具有最小分子量的氨基酸，且具有化学结构稳定，易吸收，防腐，对食盐和醋等味感起缓冲作用等优良性质，故选用甘氨酸为螯合钙的原料。
本发明目的是提供一种可靠的生物钙源螯合方法，并将甘氨酸螯合牡蛎钙添加到酱油这一大众化的调味品中，制备易于推广的高钙产品。
发明内容
本发明所要解决的技术问题一是提出一种利用生物钙源---牡蛎壳制备甘氨酸螯合钙的合成方法，二是采用此螯合钙制备高钙酱油产品。
本发明所要解决的技术问题是通过以下的技术方案实现的。本发明是一种利用生物钙源——牡蛎壳制备甘氨酸螯合钙的合成方法，其特点是：
1)牡蛎壳经清洗晾干后在800-1000℃得到灰化的牡蛎壳粉，备用。
2)称取一定比例的甘氨酸和牡蛎壳灰分，充分研磨。
3)加入温度在90～100℃范围的热水，加水量为使甘氨酸浓度为2.5％，搅拌加热条件反应30～60min。
4)反应结束后，将反应液离心，取上清液，缓慢加热浓缩近干。
5)根据氨基酸螯合物、微量的游离金属离子和氨基酸在有机溶剂中溶解度的差异，加入95％乙醇进行分离纯化，加入量约为浓缩液的5～6倍，低温4℃冷藏沉淀8h以上，弃去上清液，保留胶凝沉淀，用乙醇洗涤几次，将凝胶干燥得到产品。
本发明所得的甘氨酸螯合牡蛎钙呈白色，粉末状，无异味。将其从反应体系分离出来后，容易吸潮，易溶于水和酸，微溶于碱。其离子螯合率可达90％以上，其产率高达85％以上(以甘氨酸质量计)，实现了原料的合理充分利用。
本发明所要解决的另一技术问题是通过以下的技术方案实现的。本发明采用甘氨酸螯合牡蛎钙制备高钙酱油产品。根据甘氨酸螯合牡蛎钙在酱油中的溶解情况、风味变化及健康成人每天需钙量，经超微粉碎后直接添加到酱油中，得到高钙酱油产品。
高钙酱油主要技术指标：棕红色或红褐色澄清液体，有酱香气，鲜咸适口，可溶性无盐固形物≥8.0g/100ml，全氮(以氮计)≥0.7g/100ml，氨基态氮(以氮计)≥0.4g/100ml，钙≥200mg/100ml，卫生指标符合GB2717的规定。
具体实施方式：
实施例1。甘氨酸螯合牡蛎钙制备
牡蛎壳经清洗晾干后1000℃灰化得到牡蛎壳粉，备用。称取甘氨酸和灰分(质量比3∶1)充分研磨后，加入温度在90～100℃的热水，加水量为使甘氨酸浓度为2.5％，加热搅拌反应30min，将反应液在3000r/min转速离心15min，取上清液，缓慢加热浓缩近干，加入95％乙醇进行分离纯化，加入量约为浓缩液体积的5～6倍，低温4℃冷藏沉淀8h以上，弃去上清液，保留凝胶沉淀，用乙醇洗涤几次，烘干得到产品，干燥保藏。
实施例2。高钙酱油
每1升酱油中添加10g-20g甘氨酸螯合牡蛎钙，每人每天食用20ml此酱油，可补充人体每日所需钙的5％-10％。
Claims (2)
1.一种甘氨酸螯合牡蛎钙水相合成方法及高钙酱油的制备，其特征在于包括以下制备过程：
(1)取牡蛎壳经清洗晾晒后，充分灰化，得到含钙量较高的灰分；
(2)选用甘氨酸和步骤(1)所得的灰分为主要原料，在水相中加热搅拌反应后离心，取上清液缓慢加热浓缩至近干，加入一定体积的95％乙醇进行分离纯化后烘干，得到甘氨酸螯合牡蛎钙；
(3)根据甘氨酸螯合牡蛎钙在酱油中的溶解情况、风味变化及健康成人每天需钙量，经超微粉碎后直接添加到酱油中，得到高钙酱油。
2.根据权利要求1所述的方法，其特征在于以下几个方面：
(1)原料选用甘氨酸和经800-1000℃充分灰化的牡蛎壳粉；
(2)螯合反应条件为：灰分与甘氨酸的质量比为1∶3，加水量为保持甘氨酸浓度为2.5％，反应温度在90～100℃范围内，反应时间为30～60min，分离纯化用的95％乙醇加入量为浓缩液的5～6倍；
(3)甘氨酸螯合牡蛎钙的添加量为：每1升酱油中添加10g-20g甘氨酸螯合牡蛎钙，每人每天食用20ml此酱油，可补充人体所需钙的5％-10％。
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| CN102334690A (zh) * | 2010-07-27 | 2012-02-01 | 河北农业大学 | 一种由牡蛎壳和扇贝壳制备柠檬酸钙的方法 |
| CN102334676A (zh) * | 2010-07-27 | 2012-02-01 | 河北农业大学 | 一种胶原螯合钙的制备方法 |
| CN102442871A (zh) * | 2010-10-12 | 2012-05-09 | 青岛大学 | 以贝壳和扇贝裙边为原料的复合氨基酸螯合钙的制备方法 |
| CN110326770A (zh) * | 2019-07-31 | 2019-10-15 | 好记食品酿造股份有限公司 | 一种改进的亚麻籽饼粕酿造功能性酱油和大酱的制作方法 |
| GB202109870D0 (en) | 2020-07-08 | 2021-08-25 | Yessinergy Holding S A | Process for production of concentrates of chelated minerals |
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| CN1135852A (zh) * | 1995-05-16 | 1996-11-20 | 张昌华 | 营养保健酱油 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102334690A (zh) * | 2010-07-27 | 2012-02-01 | 河北农业大学 | 一种由牡蛎壳和扇贝壳制备柠檬酸钙的方法 |
| CN102334676A (zh) * | 2010-07-27 | 2012-02-01 | 河北农业大学 | 一种胶原螯合钙的制备方法 |
| CN102334676B (zh) * | 2010-07-27 | 2013-11-20 | 河北农业大学 | 一种胶原螯合钙的制备方法 |
| CN102442871A (zh) * | 2010-10-12 | 2012-05-09 | 青岛大学 | 以贝壳和扇贝裙边为原料的复合氨基酸螯合钙的制备方法 |
| CN110326770A (zh) * | 2019-07-31 | 2019-10-15 | 好记食品酿造股份有限公司 | 一种改进的亚麻籽饼粕酿造功能性酱油和大酱的制作方法 |
| GB202109870D0 (en) | 2020-07-08 | 2021-08-25 | Yessinergy Holding S A | Process for production of concentrates of chelated minerals |
| WO2022006649A1 (pt) | 2020-07-08 | 2022-01-13 | Yessinergy Holding S/A | Processo de produção de concentrado de minerais quelatados com aminoácidos e/ou proteínas da soja e tal produto |
| GB2601858A (en) | 2020-07-08 | 2022-06-15 | Yessinergy Holding S A | Process for production of concentrates of chelated minerals |
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| CN101747222B (zh) | 2013-02-20 |
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