CN110771892B - 一种高品质姜黄素产品、其生产方法和其应用 - Google Patents
一种高品质姜黄素产品、其生产方法和其应用 Download PDFInfo
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Abstract
本发明提供了一种高品质姜黄素产品、其生产方法和应用。所述的高品质姜黄素产品溶剂残留低、流动性好、堆积密度高。所述的生产该产品的方法,包括以下步骤:以姜黄提取物为原料,加入一定比例的结晶剂,高温溶解后继续加热或回流、降温结晶,再离心或过滤后得到姜黄素粗品,进一步烘干后,得到高品质姜黄素。所述的高品质姜黄素可作为食品、药品、饲料、化妆品等添加剂的应用。
Description
技术领域
本发明涉及一种高品质姜黄素产品、其生产方法和其应用,特别涉及一种低溶剂残留、流动性好、堆积密度高的高品质姜黄素及其制备方法和该产品在食品、饲料、药物制品和化妆品领域的应用。
背景技术
姜黄(Curcuma longa L.)属姜黄属,常用作调味与染料,是姜科姜黄属植物姜黄Curcuma longa L的干燥根茎,生长于从印度至澳大利亚,南至东亚北达浙南,在亚洲的使用历史长达千年。姜黄可提取的有效成分为姜黄素(3.5%~5%)和姜黄油(约5%),经过长达30多年的研究发现其中的姜黄素具有多种生物活性,如抗肿瘤、抗病毒、抑制阿尔茨海默、抗关节炎等活性。
目前,姜黄素常见的提取工艺有有机溶剂提取、碱水提取、酶法提取、超临界提取等,以上方法所得姜黄素粗品中常含有姜黄脂肪油、姜黄树脂等,使得姜黄素纯度较低,不易于干燥,姜黄素纯度也影响其在食品、医药中的应用。因此,姜黄素粗品还需要进一步精制,常见的精制方法包括聚酰胺吸附、大孔树脂吸附、乙酸沉淀、重结晶法等。在使用溶剂提取或结晶过程中,由于姜黄素分子结构的特殊性,导致姜黄素晶体中包裹有机溶剂,并且无法彻底脱除。市场上流通的姜黄素晶体中的有机溶剂残留均在2000-3000ppm左右,直接影响姜黄素类产品作为食品添加剂的正常使用。姜黄素可作为原料直接灌装胶囊用于膳食补充剂或药物制剂,在灌装或压片过程中对姜黄素的流动性及其堆积密度要求较高,目前姜黄素的生产工艺未注重控制结晶过程导致产品的堆积密度低、流动性差等现象,严重影响姜黄素的在医药制剂等领域的直接应用。
鉴于上述情况,为了拓宽姜黄素晶体在食品等行业的应用并克服了目前姜黄素直接应用效果不好的现状,本发明以姜黄提取物为原料,经对结晶过程的精细化控制获得了高品质姜黄素产品。
现有技术中目前存在使用重结晶方法精制、纯化姜黄素的工艺,如CN104072352A记载了通过使用生姜破碎提取工艺获得姜黄素粗品后进行了乙醇回流重结晶的步骤。此外,CN102617316A记载了姜黄经有机溶剂提取、去重金属后获得沉淀物,采用含水极性溶剂对沉淀物进行加热溶剂并室温冷却获得姜黄素结晶的方法;有报道(陈凌通,冷却结晶分离纯化姜黄素,浙江化工,2019,50(5):25-27)考察了冷却速度、搅拌方式、是否添加晶种对姜黄素结晶收率、晶体纯度的影响,公开了最优结晶条件为以10℃/min的速率下降温,磁力搅拌,加晶种。
但是,这些现有技术均未对结晶过程中的加热温度,冷却温度、搅拌速度等工艺进行考察或优化,而晶体的形成通常受外界因素干扰较大,结晶条件的多种参数都可能影响晶体的理化性质,现有技术中未公开结晶工艺中哪些具体参数对溶剂残留及晶体产物的理化性质有何具体影响,并且均没有解决改善结晶中溶剂残留和晶体堆积密度、流动性的技术问题。本发明通过溶剂的选择以及对冷却保温时间、搅拌速度、回流条件等精确参数的控制,减少了结晶产物中溶剂残留量并改善了结晶产物的堆积密度、流动性,并且该工艺方法简便、高效,适应于工业化生产,实现了为食品、药品、化妆品等领域提供高品质姜黄素添加剂的目的。
发明内容
本发明的目的是提供高品质姜黄素,其总姜黄素含量≥90%,总有机溶剂残留≤50ppm,流动性≤2.5s/g,堆积密度≥0.3g/ml,以姜黄提取物为原料经过加工处理得到。
在一些优选的实施方式中,所述高品质姜黄素总姜黄素含量在95%以上,总有机溶剂残留在30ppm以下,流动性在1.5s/g以上,堆积密度在0.4g/ml以上。
另一方面,本发明还提供了高品质姜黄素的生产方法,该方法包括以下步骤:
步骤1:溶解:以姜黄提取物为原料,加入一定比例的结晶剂,加热至溶解;
步骤2:回流:溶解的溶液在高温条件下通入惰性气体回流一定时间;
步骤3:降温结晶:溶解回流完成的姜黄提取物溶液进行降温搅拌结晶,然后在终点温度保温一定时间;
步骤4:分离、干燥:将结晶好的料液过滤或离心后得到姜黄素晶体半成品,将姜黄素晶体半成品进行干燥处理,得到高品质姜黄素。
本发明技术方案的进一步改进在于:步骤1中姜黄提取物原料是指溶剂残留小于10%的姜黄浸膏、姜黄素、姜黄油树脂,进一步优选市场上常见的溶剂残留在50~50000ppm的姜黄浸膏、姜黄素、姜黄油树脂,尤其优选50~5000ppm的姜黄浸膏、姜黄素、姜黄油树脂,最优选50~1000ppm的姜黄浸膏、姜黄素、姜黄油树脂。
本发明技术方案的进一步改进在于:步骤1中所述的结晶剂指姜黄素溶解度受温度影响明显的物质,优选C2~C4且含有1个或1个以上羟基的醇类,如乙醇、丙醇、正丙醇、异丙醇、丁醇、丙二醇、丁二醇等,尤其优选含有1~3个羟基的醇类,最优选含有1~2个羟基的醇类。
本发明技术方案的进一步改进在于:步骤1中所述的一定比例是指姜黄提取物与结晶剂的重量体积比为1:1~1:20,优选比例为1:1~1:10,尤其优选比例为1:1~1:8,最优选比例为1:3~1:5。
本发明技术方案的进一步改进在于:步骤1中所述的溶解是在原料加入结晶剂后,加热至一定温度实现的,加热温度为使结晶剂完全溶解原料且不会造成有效成分损失的任意温度。
本发明技术方案的进一步改进在于:步骤2中所述的惰性气体为除氧气以外的气体,优选的,所述惰性气体为二氧化碳或氮气。
本发明技术方案的进一步改进在于:步骤2中所述的回流时间为0.5~5h,优选回流时间0.5~3h的,尤其优选回流时间1~2h。
本发明技术方案的进一步改进在于:步骤3中所述的终点温度为0~40℃,优选温度为10~30℃,尤其优选温度为10~20℃。
本发明技术方案的进一步改进在于:步骤3中所述的搅拌转速为5~100r/min,优选转速为5~50r/min,尤其优选转速为5~30r/min。
本发明技术方案的进一步改进在于:步骤3中所述的保温时间为0~48h,优选温度为10~48h,尤其优选温度为24~48h。
本发明的最优选的技术方案为:
步骤1:溶解:以姜黄提取物为原料,加入一定比例的结晶剂,加热至溶解,结晶剂选自乙醇、丙醇、正丙醇、异丙醇、丁醇、丙二醇、丁二醇;
步骤2:回流:溶解的溶液在高温条件下通入氮气或二氧化氮加热或回流1~2h;
步骤3:降温结晶:溶解回流完成的姜黄提取物溶液进行降温搅拌结晶,然后在终点温度保温一定时间,降温的终点温度为10-20℃,搅拌速度为5-30r/min,保温时间为24-48h;
步骤4:将步骤3获得的含有结晶体的料液过滤或离心后干燥,得姜黄素提取物。
本发明的高品质姜黄素适用于食品的添加剂、饲料添加剂、作为制备药品和化妆品和制备食品添加剂产品的组分。
在食品领域中典型的使用方面是例如功能饮料、奶制品、冰淇淋的着色和奶粉、蛋产品、烘烤混合物和糖食的着色。
在饲料领域中,姜黄素可被用于例如在家禽饲养中、宠物功能饲料添加剂。
在化妆品领域,姜黄素可用于例如作为用于装饰性的身体护理组合物的着色剂。
在药品领域,姜黄素可用于药物制剂尤其是片剂、包衣片和胶囊。
本发明的有益效果在于:本发明通过结晶控制,有效降低了姜黄素中的溶剂残留,提高了姜黄素的流动性,使姜黄素可以直接作为食品添加剂在食品中应用;整个工艺处理过程中,姜黄素的有效含量损失低于5%,可以有效提高姜黄素的单位纯度至90%以上;工艺过程只使用醇类溶剂,有效的提高了生产过程的安全性及食品安全;操作相对简单,易于实现规模化生产。
具体实施方式
下面通过具体的实施方案叙述本发明方法。另外,实施方案应理解为说明性的,而非限制本发明的范围,本发明的实质和范围仅由权利要求书所限定。
实施例中原料姜黄提取物和产品姜黄素的溶剂残留按《GB1886.76–2016》的检测方法进行测定。
姜黄素产品的流动性使用粉末流动仪(霍尔流速计)进行测定。本申请所述的姜黄素流动性是以一定量姜黄素流过规定孔径的标准漏斗所需要的时间来表示,采用的单位为s/g,该数值越低表明粉末的流动性越好。
姜黄素产品的堆积密度按照《GB/T 20316.2-2006》的检测方法进行测定。
产品中姜黄素含量按照《美国药典USP39—姜黄素》的检测方法进行测定。
实施例1
溶解:取溶剂残留为5%(质量分数)的姜黄浸膏原料100g,加入100ml的正丁醇,升温至115℃,搅拌溶解;
回流:在117℃条件下通入二氧化碳,回流0.5h后开始降温;
降温结晶:回流完的溶液进行降温搅拌结晶,搅拌转速为100r/min,温度降至40℃后保温48h;
分离、干燥:将结晶好的料液抽滤后得到姜黄素晶体半成品,将姜黄素晶体半成品进行干燥处理,得到高品质姜黄素。
通过以上高品质姜黄素的生产方法,得到的姜黄素溶残为48ppm,姜黄素的流动性为2.5s/g,堆积密度为0.32g/ml,姜黄素含量为90.3%。
实施例2
溶解:取溶剂残留为1%(质量分数)的姜黄浸膏原料200g,加入400ml的丙二醇,升温至150℃,搅拌溶解;
回流:在150℃条件下通入二氧化碳,加热1h后开始降温;
降温结晶:回流完的溶液进行降温搅拌结晶,搅拌转速为50r/min,温度降至30℃后保温24h;
分离、干燥:将结晶好的料液抽滤后得到姜黄素晶体半成品,将姜黄素晶体半成品进行干燥处理,得到高品质姜黄素。
通过以上高品质姜黄素的生产方法,得到的姜黄素溶残为42ppm,姜黄素的流动性为2.0s/g,堆积密度为0.37g/ml,姜黄素含量为93.7%。
实施例3
溶解:取溶剂残留为5000ppm的姜黄提取物原料150g,加入1500ml的乙醇,升温至78℃,搅拌溶解;
回流:在75℃条件下通入氮气,回流2h后开始降温;
降温结晶:回流完的溶液进行降温搅拌结晶,搅拌转速为30r/min,温度降至20℃后保温12h;
分离、干燥:将结晶好的料液抽滤后得到姜黄素晶体半成品,将姜黄素晶体半成品进行干燥处理,得到高品质姜黄素。
通过以上高品质姜黄素的生产方法,得到的姜黄素溶残为30ppm,姜黄素的流动性为1.5s/g,堆积密度为0.45g/ml,姜黄素含量为95.6%。
实施例4
溶解:取溶剂残留为1000ppm的姜黄提取物原料100g,加入2000ml的异丙醇,升温至82℃,搅拌溶解;
回流:在82℃条件下通入二氧化碳,回流5h后开始降温;
降温结晶:回流完的溶液进行降温搅拌结晶,搅拌转速为10r/min,温度降至10℃后保温1h;
分离、干燥:将结晶好的料液抽滤后得到姜黄素晶体半成品,将姜黄素晶体半成品进行干燥处理,得到高品质姜黄素。
通过以上高品质姜黄素的生产方法,得到的姜黄素溶残为25ppm,姜黄素的流动性为1.0s/g,堆积密度为0.50g/ml,姜黄素含量为97.0%。
实施例5
溶解:取溶剂残留为50ppm的姜黄提取物原料100g,加入500ml的丙二醇,升温至100℃,搅拌溶解;
回流:在100℃条件下通入氮气,加热5h后开始降温;
降温结晶:回流完的溶液进行降温搅拌结晶,搅拌转速为5r/min,温度降至15℃后保温12h;
分离、干燥:将结晶好的料液抽滤后得到姜黄素晶体半成品,将姜黄素晶体半成品进行干燥处理,得到高品质姜黄素。
通过以上高品质姜黄素的生产方法,得到的姜黄素溶残为15ppm,姜黄素的流动性为0.5s/g,堆积密度为0.55g/ml,姜黄素含量为98.7%。
对比实验:
除表1中所列明确列出的实验参数值,对比例1-7其他实验参数均与实施例3的条件参数相同,表1显示了不同实验条件下所获的的姜黄提取物的性能指标。
表1
从上述对比例可以看出,本申请所要求保护的各项结晶条件参数的选择对结晶物中溶剂残留量、流动性和堆积密度产生了明显的改善作用。
虽然,上文中已经用一般性说明、具体实施方式及试验,对本发明作了详尽的描述,但在本发明基础上,可以对之作一些修改或改进,这对本领域技术人员而言是显而易见的。因此,在不偏离本发明精神的基础上所做的这些修改或改进,均属于本发明要求保护的范围。
Claims (12)
1.一种姜黄素提取物,其特征在于:总姜黄素含量不低于90%,总溶剂残留不高于50ppm,流动性不高于2.5s/g,堆积密度不低于0.3g/ml,该姜黄素提取物的制备包括以下工艺步骤:步骤1:溶解:以姜黄提取物为原料,加入一定比例的结晶剂,加热至溶解;步骤2:回流:溶解的溶液在高温条件下通入惰性气体加热或回流一定时间;步骤3:降温结晶:溶解回流完成的姜黄提取物溶液进行降温搅拌结晶,然后在终点温度保温一定时间,保温结束后将含有结晶体的料液过滤或离心后干燥获得姜黄素提取物;步骤1中姜黄提取物原料是指溶剂残留小于10%(质量分数)的姜黄浸膏、姜黄素、或姜黄油树脂;步骤1所述结晶选自乙醇、丙醇、正丁醇、异丙醇、丁醇、丙二醇、丁二醇的一种或多种,步骤1中所述的一定比例是指姜黄提取物与结晶剂的重量体积比为1:1~1:20;步骤3中所述的终点温度为0~40℃。
2.根据权利要求1所述的姜黄素提取物,其特征在于:步骤1中姜黄提取物原料是指市场上常见的溶剂残留在50~50000ppm的姜黄浸膏、姜黄素、姜黄油树脂。
3.根据权利要求1所述的姜黄素提取物,其特征在于:步骤1中姜黄提取物与结晶剂的重量体积比为1:1~1:10。
4.根据权利要求3所述的姜黄素提取物,其特征在于:步骤1中姜黄提取物与结晶剂的重量体积比1:3~1:5。
5.根据权利要求1所述的姜黄素提取物,其特征在于:步骤2中所述的惰性气体为二氧化碳或氮气。
6.根据权利要求1所述的姜黄素提取物,其特征在于:步骤2中所述的加热或回流时间为0.5~5h。
7.根据权利要求1所述的姜黄素提取物,其特征在于:步骤3中所述的终点温度为10~30℃。
8.根据权利要求7所述的姜黄素提取物,其特征在于:步骤3中所述的终点温度为10-20℃。
9.根据权利要求1所述的姜黄素提取物,其特征在于:步骤3中所述的搅拌转速为5~100r/min。
10.根据权利要求1所述的姜黄素提取物,其特征在于:步骤3中所述的保温时间为0~48h。
11.一种组合物,其中包含权利要求1-10任一项所述姜黄素提取物。
12.权利要求1-11任一项所述姜黄素提取物作为食品、饲料、药物制品和化妆品的功能性添加剂或着色剂应用。
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