CN110477395A - 一种类胡萝卜素制剂的制备方法 - Google Patents
一种类胡萝卜素制剂的制备方法 Download PDFInfo
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- CN110477395A CN110477395A CN201910702395.2A CN201910702395A CN110477395A CN 110477395 A CN110477395 A CN 110477395A CN 201910702395 A CN201910702395 A CN 201910702395A CN 110477395 A CN110477395 A CN 110477395A
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- A—HUMAN NECESSITIES
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- A—HUMAN NECESSITIES
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- A—HUMAN NECESSITIES
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- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
本发明涉及一种类胡萝卜素制剂的制备方法,该方法的步骤如下:1)将类胡萝卜素和其它原料加入纯净水中,搅拌溶解并乳化均匀;2)将所述步骤1)中制备所得物料转入研磨设备中研磨,取样测粒径为0.01~2μm;3)将所述步骤2)中粒径为0.01~2μm所得物料喷雾干燥,通过淀粉包埋二次制粒,得到类胡萝卜素微胶囊。该方法中有效避免有机溶剂在微胶囊上的残留,无溶剂残留风险;并且不需要在高温高压的条件下进行制备,提高了产率,而且工艺简单,改善了制备条件,优化生产工艺,有利于产品的产业化生产。
Description
技术领域
本发明涉及医药食品加工技术领域,尤其涉及一种类胡萝卜素制剂的制备方法。
背景技术
类胡萝卜素是一类带有多个不饱和键的多烯化合物,其可以用作食品中的功能性保健成分或着色剂,如α-胡萝卜素或β-胡萝卜素、8'-阿朴-β-胡萝卜醛、8'-阿朴-β-胡萝卜酸乙基酯、角黄素、虾青素、番茄红素、叶黄素、玉米黄质或藏红花素等。目前,类胡萝卜素制剂的制备主要采用两种方法:一种是采用溶剂溶解,在后续过程中将溶剂去除,此方法由于采用有机溶剂,使产品存在溶剂残留的风险;另一种是在高温高压的条件下采用熔融的方式处理,生产条件苛刻,并且在高温条件下,类胡萝卜素会发生不同程度的氧化,从而导致产品的收率降低。
发明内容
有鉴于此,有必要针对的问题,提供一种类胡萝卜素制剂的制备方法,旨在改善制备条件,优化生产工艺,不存在溶剂残留风险,同时提高产品收率。
为解决上述技术问题,本发明提出一种类胡萝卜素制剂的制备方法,该方法步骤如下:
1)将类胡萝卜素和其它原料加入纯净水中,搅拌溶解并乳化均匀;
2)将所述步骤1)中制备所得物料转入研磨设备中研磨,取样测粒径为0.01~2μm;
3)将所述步骤2)中粒径为0.01~2μm所得物料喷雾干燥,通过淀粉包埋二次制粒,得到类胡萝卜素微胶囊。
可选地,所述步骤1)中的所述其它原料包括壁材和抗氧化剂,且各组分按重量份计,所述类胡萝卜素1份、所述壁材3~98份、所述抗氧化剂0.1~0.8份、所述纯净水3~98份。
可选地,所述壁材采用阿拉伯胶、改性淀粉、木质素磺酸钠、木质素磺酸钙、聚丙烯酸钠和羧甲基纤维素钠中的一种或几种。
可选地,所述抗氧化剂采用抗坏血酸、抗坏血酸钠、维生素E、2,6-二叔丁基-4-甲基苯酚、丁基羟基茴香醚和抗坏血酸棕榈酸酯中的一种或几种。
可选地,所述步骤2)中采用所述研磨设备的研磨条件为:转速100~5000转/分钟,球磨筛网由粗至细分为2~30级,每级研磨5~45分钟,总研磨时间为30~300分钟。
可选地,所述研磨设备的总研磨时间为60~180分钟。
可选地,所述步骤3)中所述喷雾干燥的条件为:进风温度110℃,进料速度120ml/min。
本发明通过采用类胡萝卜素和其它原料在纯净水中搅拌混合、乳化均匀,并通过研磨使取样测粒径为0.01~2μm,再通过喷雾干燥、淀粉包埋二次制粒的制备方法,制备得到类胡萝卜素微胶囊。该方法中不采用有机溶剂,有效避免有机溶剂在微胶囊上的残留,无溶剂残留风险,充分保障产品的食用安全。并且主要采用研磨的方式获得微颗粒,不需要在高温高压的条件下进行制备,从而避免类胡萝卜素在高温高压条件下的分解,提高了产率,而且改善了制备条件,优化生产工艺,工艺简单,有利于产品的产业化生产。
具体实施方式
下面将结合本发明的具体实施例对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
以下实施例中,类胡萝卜素采用的是β-胡萝卜素、8'-阿朴-β-胡萝卜醛、8'-阿朴-β-胡萝卜酸乙基酯、角黄素、番茄红素、叶黄素和玉米黄质的一种或几种;壁材采用的是阿拉伯胶、改性淀粉、木质素磺酸钠、木质素磺酸钙、聚丙烯酸钠和羧甲基纤维素钠中的任意一种或几种;抗氧化剂采用的是抗坏血酸、抗坏血酸钠、维生素E、2,6-二叔丁基-4-甲基苯酚(简称BHT)、丁基羟基茴香醚(简称BHA)和抗坏血酸棕榈酸酯中的一种或几种。
研磨设备的研磨条件为:转速100~5000转/分钟,球磨筛网由粗至细分为2~30级,每级研磨5~45min,总研磨时间为30min~300min。研磨设备采用研磨机、砂磨机、胶体磨、珠磨机,当然也可采用其他研发设备,在此不做具体限定。
实施例一
本实施例中一种类胡萝卜素制剂的制备方法,该方法步骤如下:
1)将番茄红素晶体(含量98%)1份、阿拉伯胶3份、抗坏血酸0.1份加入3份纯净水中,搅拌溶解并乳化均匀;
2)将步骤1)中制备所得物料转入研磨设备中研磨,由粗至细,分2级研磨,每级研磨15min,共研磨30min,取样马尔文3000测定粒径为2.02μm;
3)将步骤2)中粒径为2.02μm所得物料在进风温度110℃,进料速度120ml/min的条件下喷雾干燥,通过淀粉包埋二次制粒,得到番茄红素微胶囊。
实施例二
本实施例中一种类胡萝卜素制剂的制备方法,该方法步骤如下:
1)将β-胡萝卜素晶体(含量98%)1份、改性淀粉5份、抗坏血酸钠0.2份加入12.5份纯净水中,搅拌溶解并乳化均匀;
2)将步骤1)中制备所得物料转入研磨设备中研磨,由粗至细,分5级研磨,每级研磨30min,共研磨150min,取样马尔文3000测定粒径为0.185μm;
3)将步骤2)中粒径为0.185μm所得物料在进风温度110℃,进料速度120ml/min的条件下喷雾干燥,通过淀粉包埋二次制粒,得到β-胡萝卜素微胶囊。
实施例三
本实施例中一种类胡萝卜素制剂的制备方法,该方法步骤如下:
1)将8'-阿朴-β-胡萝卜醛晶体1份、木质素磺酸钠10份、维生素E 0.3份加入15份纯净水中,搅拌溶解并乳化均匀;
2)将步骤1)中制备所得物料转入研磨设备中研磨,由粗至细,分8级研磨,每级研磨20min,共研磨160min,取样马尔文3000测定粒径为0.172μm;
3)将步骤2)中粒径为0.172μm所得物料在进风温度110℃,进料速度120ml/min的条件下喷雾干燥,通过淀粉包埋二次制粒,得到8'-阿朴-β-胡萝卜醛微胶囊。
实施例四
本实施例中一种类胡萝卜素制剂的制备方法,该方法步骤如下:
1)将8'-阿朴-β-胡萝卜酸乙基酯1份、木质素磺酸钙20份、BHT0.4份加入20份纯净水中,搅拌溶解并乳化均匀;
2)将步骤1)中制备所得物料转入研磨设备中研磨,由粗至细,分10级研磨,每级研磨20min,共研磨200min,取样马尔文3000测定粒径为0.205μm;
3)将步骤2)中粒径为0.205μm所得物料在进风温度110℃,进料速度120ml/min的条件下喷雾干燥,通过淀粉包埋二次制粒,得到8'-阿朴-β-胡萝卜酸乙基酯微胶囊。
实施例五
本实施例中一种类胡萝卜素制剂的制备方法,该方法步骤如下:
1)将角黄素1份、聚丙烯酸钠40份、BHA0.5份加入30份纯净水中,搅拌溶解并乳化均匀;
2)将步骤1)中制备所得物料转入研磨设备中研磨,由粗至细,分15级研磨,每级研磨20min,共研磨300min,取样马尔文3000测定粒径为0.011μm;
3)将步骤2)中粒径为0.011μm所得物料在进风温度110℃,进料速度120ml/min的条件下喷雾干燥,通过淀粉包埋二次制粒,得到角黄素微胶囊。
实施例六
本实施例中一种类胡萝卜素制剂的制备方法,该方法步骤如下:
1)将叶黄素1份、羧甲基纤维素钠70份、抗坏血酸棕榈酸酯0.6份加入60份纯净水中,搅拌溶解并乳化均匀;
2)将步骤1)中制备所得物料转入研磨设备中研磨,由粗至细,分20级研磨,每级研磨5min,共研磨100min,取样马尔文3000测定粒径为1.21μm;
3)将步骤2)中粒径为1.21μm所得物料在进风温度110℃,进料速度120ml/min的条件下喷雾干燥,通过淀粉包埋二次制粒,得到类胡萝卜素微胶囊。
实施例七
本实施例中一种类胡萝卜素制剂的制备方法,该方法步骤如下:
1)将玉米黄质1份、改性淀粉80份、抗坏血酸棕榈酸酯0.7份加入80份纯净水中,搅拌溶解并乳化均匀;
2)将步骤1)中制备所得物料转入研磨设备中研磨,由粗至细,分2级研磨,每级研磨45min,共研磨90min,取样马尔文3000测定粒径为1.7μm;
3)将步骤2)中粒径为1.7μm所得物料在进风温度110℃,进料速度120ml/min的条件下喷雾干燥,通过淀粉包埋二次制粒,得到玉米黄质微胶囊。
实施例八
本实施例中一种类胡萝卜素制剂的制备方法,该方法步骤如下:
1)将β-胡萝卜素晶体(含量98%)1份、改性淀粉98份、抗坏血酸棕榈酸酯0.8份加入98份纯净水中,搅拌溶解并乳化均匀;
2)将步骤1)中制备所得物料转入研磨设备中研磨,由粗至细,分30级研磨,每级研磨10min,共研磨300min,取样马尔文3000测定粒径为0.82μm;
3)将步骤2)中粒径为0.82μm所得物料在进风温度110℃,进料速度120ml/min的条件下喷雾干燥,通过淀粉包埋二次制粒,得到β-胡萝卜素微胶囊。
对比实施例
本实施例中一种类胡萝卜素制剂的制备方法,该方法步骤如下:
1)将β-胡萝卜素1份、改性淀粉40份、抗坏血酸棕榈酸酯0.5份加入40份纯净水中,搅拌溶解并乳化均匀;
2)将改性淀粉40份、抗坏血酸棕榈酸酯0.3份及60份纯净水搅拌溶解乳化,置于冰水循环系统中降温至3±1℃并保持,
3)将步骤1)中制备所得物料转入三级升温加压熔融系统中熔融,三级温度分别为80℃、120℃、155℃,对应三级温度的加压压力分别为20Mpa、40Mpa、60Mpa,各级停留加热时间均为15秒钟;
4)将步骤3)中所得物料迅速转入步骤2)中物料中,转入过程中快速搅拌,使步骤3)中物料快速均匀分散于步骤2)的物料中,转料完毕后再高速搅拌5分钟后取样,马尔文3000测定粒径为0.01μm;
5)将步骤4)所得物料在进风温度110℃,进料速度120ml/min的条件下喷雾干燥,通过淀粉包埋二次制粒,得到β-胡萝卜素微胶囊。
结果测试
以类胡萝卜素的原料质量计算:
产品收率=(类胡萝卜素微胶囊质量×类胡萝卜素微胶囊中类胡罗卜素含量)/(类胡萝卜素原料质量×类胡罗卜素原料含量)×100%
结果如下:
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (7)
1.一种类胡萝卜素制剂的制备方法,其特征在于,该方法步骤如下:
1)将类胡萝卜素和其它原料加入纯净水中,搅拌溶解并乳化均匀;
2)将所述步骤1)中制备所得物料转入研磨设备中研磨,取样测粒径为0.01~2μm;
3)将所述步骤2)中粒径为0.01~2μm所得物料喷雾干燥,通过淀粉包埋二次制粒,得到类胡萝卜素微胶囊。
2.如权利要求1所述的类胡萝卜素制剂的制备方法,其特征在于,所述步骤1)中的所述其它原料包括壁材和抗氧化剂,且各组分按重量份计,所述类胡萝卜素1份、所述壁材3~98份、所述抗氧化剂0.1~0.8份、所述纯净水3~98份。
3.如权利要求2所述的类胡萝卜素制剂的制备方法,其特征在于,所述壁材采用阿拉伯胶、改性淀粉、木质素磺酸钠、木质素磺酸钙、聚丙烯酸钠和羧甲基纤维素钠中的一种或几种。
4.如权利要求2所述的类胡萝卜素制剂的制备方法,其特征在于,所述抗氧化剂采用抗坏血酸、抗坏血酸钠、维生素E、2,6-二叔丁基-4-甲基苯酚、丁基羟基茴香醚和抗坏血酸棕榈酸酯中的一种或几种。
5.如权利要求1所述的类胡萝卜素制剂的制备方法,其特征在于,所述步骤2)中采用所述研磨设备的研磨条件为:转速100~5000转/分钟,球磨筛网由粗至细分为2~30级,每级研磨5~45分钟,总研磨时间为30~300分钟。
6.如权利要求5所述的类胡萝卜素制剂的制备方法,其特征在于,所述研磨设备的总研磨时间为60~180分钟。
7.如权利要求1所述的类胡萝卜素制剂的制备方法,其特征在于,所述步骤3)中所述喷雾干燥的条件为:进风温度110℃,进料速度120ml/min。
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