CN112155210B - 一种栀子油纳米乳液冻干粉及其制备方法 - Google Patents
一种栀子油纳米乳液冻干粉及其制备方法 Download PDFInfo
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Classifications
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- A—HUMAN NECESSITIES
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- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23L3/40—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- Edible Oils And Fats (AREA)
Abstract
本发明公开了一种栀子油纳米乳液冻干粉及其制备方法,结合真空冷冻干燥技术和动态微射流技术制备。将藏红花酸溶于栀子油作为油相;乳清分离蛋白或大豆分离蛋白分散于磷酸盐缓冲溶液中,获得蛋白溶液作为水相;在高速分散条件下向水相中加入油相,形成初乳;初乳经动态高压微射流技术处理得到单层栀子油纳米乳;单层栀子油纳米乳中加入阴离子多糖溶液经动态高压微射流技术处理形成双层栀子油纳米乳,真空冷冻干燥得到栀子油纳米乳液冻干粉。本发明开发出一种新型的蛋白质‑多糖修饰技术的双层纳米乳液冻干粉,用于生产粒径更小、稳定性更高的富含藏红花酸栀子油载体,操作简便,能够进行连续生产,能够被广泛应用到饮料的生产中。
Description
技术领域
本发明属于食品药品技术领域,具体涉及可食用栀子油。
背景技术
栀子是目前常见大宗药材之一,来源于茜草科植物栀子Gardenia jasminoidesEllis的干燥成熟果实,主产于福建、江西、湖南、浙江等省。栀子性苦、味寒,具有泻火除烦、凉血解毒的功效,主要含有环烯醚萜类、有机酸类和栀子黄色素等成分。现代药理研究,栀子具有抗氧化、抗炎镇痛、抗微生物、保肝利胆、降血糖等作用。栀子成熟果实中含有大量的油类成分,含油量在15%~20%,且栀子油中脂肪酸含量达到80%左右,主要是亚油酸及油酸。现代药理学研究表明,栀子油中所含的不饱和脂肪酸、甾醇、谷维素、维生素E等成分,具有保肝、降血脂、抗肿瘤、镇静催眠、抗衰老及促进学习记忆的作用。但栀子油中多不饱和脂肪酸、藏红花酸和藏红花素含量丰富,极易受环境中的空气、光照和水的影响而发生氧化、酸败并产生醛酮类等有害物质,稳定性差,使得栀子油的产品形式和推广应用受到极大限制。
纳米乳液(nanoemulsion)是由水相、油相、表面活性剂等多组分混合而成的热力学稳定的胶体分散体系,液滴粒度一般在100~200nm。目前,纳米乳液由于粒度较小且尺度均一、稳定性较好、黏度较低等优点,解决了油溶性功能成分水溶性差、易氧化、难吸收等问题,在食品药品领域已引起广泛关注。但截至目前还未有一种栀子油纳米乳液制品的报道。
发明内容
本发明的目的在于克服现有技术的不足之处,提供了一种栀子油纳米乳液冻干粉及其制备方法,以栀子油和藏红花酸为主要原料,先通过乳清分离蛋白或大豆分离蛋白以及添加了藏红花酸的栀子油经过动态高压微射流技术制备单层栀子油纳米乳,再添加羧甲基纤维素钠或阿拉伯胶经过动态高压微射流技术得到双层栀子油纳米乳,真空冷冻干燥制备出所需的栀子油纳米乳液冻干粉。
本发明解决其技术问题所采用的技术方案之一是:
一种栀子油纳米乳液冻干粉的制备方法,包括:
1)以蛋白的溶液作为水相,以添加了藏红花酸的栀子油作为油相,将油相加入到水相中,在24000~28000r/min分散5~10min,形成初乳;
2)将所述初乳通过动态高压微射流技术(dynamic high pressuremicrofluidization,DHPM)均质处理3~6次,均质压力为50~80MPa,得到单层栀子油纳米乳;
3)向所述单层栀子油纳米乳中加入阴离子多糖的溶液,通过动态高压微射流技术均质处理5~6次,均质压力为60~90MPa,得到双层栀子油纳米乳;
4)所述双层栀子油纳米乳冷冻干燥,得到所述栀子油纳米乳液冻干粉。
一实施例中,所述蛋白包括乳清分离蛋白或大豆分离蛋白中的至少一种。
一实施例中,所述阴离子多糖包括羧甲基纤维素钠或阿拉伯胶中的至少一种。
一实施例中,所述步骤1)中,所述栀子油的制备方法包括:栀子剥皮果在CO2流量25~45L/h,压力10~35MPa,温度35~65℃下进行超临界CO2萃取0.5~6h,得到所述栀子油。
一实施例中,所述步骤1)中,所述水相的制备方法包括:将蛋白按照1:20~1:10的料液比(g:mL)分散于pH 6.8~7.2的磷酸盐缓冲溶液中,室温下搅拌4~6小时后,0~5℃溶胀12~24h,得到所述水相。
进一步地,所述磷酸盐缓冲溶液的浓度为0.05~0.1M。
一实施例中,所述油相中,藏红花酸与栀子油的质量比为0.04~0.06:100。
进一步地,所述油相的制备方法包括:采用超声处理20~30min至藏红花酸完全溶解于栀子油,超声处理的温度为20~40℃,超声功率为100~300W。
一实施例中,所述步骤1)中,采用高速分散机(如D-500,北京大龙仪器有限公司)进行分散处理。
一实施例中,所述步骤2)和步骤3)中,采用动态高压微射流纳米均质机(如AH-1500,加拿大ATS公司)进行均质处理。
一实施例中,所述步骤3)中,所述阴离子多糖在所述双层栀子油纳米乳中的最终质量浓度为0.4~1.0g/100mL。
一实施例中,所述步骤4)中,所述冷冻干燥为-85~-75℃冷冻干燥45~50h。
本发明解决其技术问题所采用的技术方案之二是:
一种根据上述的制备方法所制备的栀子油纳米乳液冻干粉。
本发明所得栀子油纳米乳液冻干粉的颗粒小于152.6nm,基本分布在100~120nm左右,藏红花酸包埋率达到90%以上,而且加热稳定性达到90%以上,储藏稳定性达到90%以上。本发明将栀子油制备成纳米乳液,不仅可以防止其中不饱和脂肪酸过早氧化生成对人体有害的物质,也可提高栀子油的生物利用度和环境耐受性,解决栀子油的稳定性问题,进而使得栀子油充分发挥其营养价值。
本发明所涉及的设备、试剂、工艺、参数等,除有特别说明外,均为常规设备、试剂、工艺、参数等,不再作实施例。
本发明所列举的所有范围包括该范围内的所有点值。
本发明所述“大约”、“约”或“左右”等指的是所述范围或数值的±10%范围内。
本发明中,所述“室温”即常规的室内环境温度,可以为10~30℃。
本技术方案与背景技术相比,它具有如下优点:
(1)本发明利用高压微射流处理技术,通过蛋白质先进行单层栀子油纳米乳制备,再通过阴离子多糖进行双层栀子油纳米乳制备,经过两层包埋,有效提高了栀子油纳米乳液稳定性,制备出稳定性和包埋率均高的双层纳米乳液。
(2)本发明中牛乳清分离蛋白或大豆分离蛋白作为天然食品蛋白,成本较低,具有生物相容性、生物降解性等良好功能性质。
(3)本发明中为了提高纳米乳液的稳定性,添加了与蛋白质所带电荷相反的阴离子多糖,如阿拉伯胶或羧甲基纤维素钠,利用动态高压微射流技术和静电结合形成双层栀子油纳米乳,从而提高蛋白乳液在极端环境下的稳定性。
(4)本发明中通过真空冷冻干燥技术得到栀子油纳米乳液冻干粉具有致密、均匀的结构和光滑平整的表面,能够留存藏红花酸和栀子油的色泽、香味和营养成分,同时冻干粉具有速溶性和水复溶性,提高了藏红花酸和不饱和脂肪酸组分的稳定性。
(5)本发明联合真空冷冻干燥技术、动态微射流技术、蛋白质和阴性多糖电荷结合、双层纳米乳液制备技术,制备得到高稳定性和良好复溶性的栀子油纳米乳液冻干粉末,提高了藏红花酸和栀子油的稳定性和生物利用度。
(6)本发明中栀子油与藏红花酸组分配合,其一藏红花酸与栀子油共同属于栀子中原有成分,保存栀子成分完整性;其二藏红花酸具有抗氧化、抗血小板聚集、抗动脉粥样硬化、改善心肌肥厚、预防心肌缺血和再灌注损伤、降低血压和心脏保护作用、预防急性低氧性脑损伤、预防脑缺血再灌注损伤等治疗心脑血管疾病方面药理活性。本发明通过在栀子油中添加藏红花酸,提高了栀子油的抗氧化活性,同时也具有改善心脑血管系统疾病、保护心脑血管功效。
(7)本发明所涉及的生产过程简便、快捷,不涉及有害的化学试剂,具有工业化和规模化的前景,适合于生产富含高藏红花酸的栀子油的功能性食品、药品等领域。
具体实施方式
下面通过实施例具体说明本发明的内容:
粒度和分散性测试方法:将对比例或实施例中制备的样品稀释至栀子油纳米乳液冻干粉或纳米乳浓度约为10mg/mL后,采用动态光散射法DLS测定纳米颗粒的平均粒径和分散性,结果取三次测定的平均值。
藏红花酸包埋率测定方法:采用高效液相色谱法测定藏红花酸包埋率,具体操作方法如下:
色谱条件:ODS-C18色谱柱(250mm×4.6mm,5μm),甲醇:2%甲酸溶液=70:30;柱温:室温,波长:430nm。
加热稳定性测试方法:将对比例或实施例中制备的栀子油纳米乳液冻干粉或纳米乳于60℃下储藏48小时后,测定其藏红花酸含量,加热稳定性按以下公式计算:
加热稳定性(%)=(60℃下储藏48小时后纳米乳液冻干粉或纳米乳中的藏红花酸含量/新鲜纳米乳液冻干粉或纳米乳中藏红花酸含量)×100%
储藏稳定性测试方法:将对比例或实施例中制备的栀子油纳米乳液冻干粉或纳米乳于室温下储藏两个月后,测定其藏红花酸含量,储存稳定性按以下公式计算:
储藏稳定性(%)=(储藏两个月后纳米乳液冻干粉或纳米乳中的藏红花酸含量/新鲜纳米乳液冻干粉或纳米乳中藏红花酸含量)×100%
实施例1
1)栀子剥皮果在CO2流量25L/h,压力25MPa,温度50℃下进行超临界CO2萃取2h,得到栀子油;
2)将乳清分离蛋白溶于pH 7.0的0.1M磷酸盐缓冲溶液中,乳清分离蛋白与磷酸盐缓冲溶液料液比为1:10(质量/体积,g:mL),室温下搅拌4小时后,于4℃下冷藏保存,溶胀达24h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率150W,超声温度30℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(24000r/min,10min),将油相缓慢加入到水相中,形成初乳;
5)将制备好的初乳样品通过动态高压微射流纳米均质机(AH-1500,加拿大ATS公司),经过6次均质、均质压力为50MPa,得到单层栀子油纳米乳;
6)加入一定浓度的羧甲基纤维素钠溶液于单层栀子油纳米乳中,进行均质,经过6次均质、均质压力为80MPa,得到双层栀子油纳米乳,羧甲基纤维素钠在双层栀子油纳米乳中最终质量浓度为0.4g/100mL。
7)双层栀子油纳米乳,冷冻干燥48h,冷冻温度为-80℃,得到栀子油纳米乳液冻干粉。所得栀子油纳米乳液冻干粉中,颗粒平均粒径115.7nm,藏红花酸包埋率94%,加热稳定性96%,储藏稳定性98%。
实施例2
1)栀子剥皮果在CO2流量25L/h,压力25MPa,温度50℃下进行超临界CO2萃取2h,得到栀子油;
2)将乳清分离蛋白溶于pH 7.0的0.1M磷酸盐缓冲溶液中,乳清分离蛋白与磷酸盐缓冲溶液料液比为1:20(质量/体积,g:mL),室温下搅拌4小时后,于4℃下冷藏保存,溶胀达24h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率300W,超声温度30℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(24000r/min,10min),将油相缓慢加入到水相中,形成初乳;
5)将制备好的初乳样品通过动态高压微射流纳米均质机(AH-1500,加拿大ATS公司),经过6次均质、均质压力为50MPa,得到单层栀子油纳米乳;
6)加入一定浓度的羧甲基纤维素钠溶液于单层栀子油纳米乳中,进行均质,经过6次均质、均质压力为80MPa,得到双层栀子油纳米乳,羧甲基纤维素钠在双层栀子油纳米乳中最终质量浓度为0.4g/100mL。
7)双层栀子油纳米乳,冷冻干燥48h,冷冻温度为-80℃,得到栀子油纳米乳液冻干粉。所得栀子油纳米乳液冻干粉中,颗粒平均粒径110.1nm,藏红花酸包埋率94.6%,加热稳定性95.7%,储藏稳定性97.3%。
实施例3
1)栀子剥皮果在CO2流量25L/h,压力25MPa,温度50℃下进行超临界CO2萃取2h,得到栀子油;
2)将乳清分离蛋白溶于pH 7.0的0.1M磷酸盐缓冲溶液中,乳清分离蛋白与磷酸盐缓冲溶液料液比为1:10(质量/体积,g:mL),室温下搅拌4小时后,于4℃下冷藏保存,溶胀达24h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率150W,超声温度30℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(24000r/min,10min),将油相缓慢加入到水相中,形成初乳;
5)将制备好的初乳样品通过动态高压微射流纳米均质机(AH-1500,加拿大ATS公司),经过6次均质、均质压力为60MPa,得到单层栀子油纳米乳;
6)加入一定浓度的羧甲基纤维素钠溶液于单层栀子油纳米乳中,进行均质,经过6次均质、均质压力为80MPa,得到双层栀子油纳米乳,羧甲基纤维素钠在双层栀子油纳米乳中最终质量浓度为0.4g/100mL。
7)双层栀子油纳米乳,冷冻干燥48h,冷冻温度为-80℃,得到栀子油纳米乳液冻干粉。所得栀子油纳米乳液冻干粉中,颗粒平均粒径102.6nm,藏红花酸包埋率94%,加热稳定性97%,储藏稳定性95%。
实施例4
1)栀子剥皮果在CO2流量25L/h,压力25MPa,温度50℃下进行超临界CO2萃取2h,得到栀子油;
2)将大豆分离蛋白溶于pH 7.0的0.1M磷酸盐缓冲溶液中,大豆分离蛋白与磷酸盐缓冲溶液料液比为1:15(质量/体积,g:mL),室温下搅拌4小时后,于4℃下冷藏保存,溶胀达24h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率150W,超声温度30℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(24000r/min,5min),将油相缓慢加入到水相中,形成初乳;
5)将制备好的初乳样品通过动态高压微射流纳米均质机(AH-1500,加拿大ATS公司),经过6次均质、均质压力为50MPa,得到单层栀子油纳米乳;
6)加入一定浓度的羧甲基纤维素钠溶液于单层栀子油纳米乳中,进行均质,经过6次均质、均质压力为80MPa,得到双层栀子油纳米乳,羧甲基纤维素钠在双层栀子油纳米乳中最终质量浓度为0.4g/100mL。
7)双层栀子油纳米乳,冷冻干燥48h,冷冻温度为-80℃,得到栀子油纳米乳液冻干粉。所得栀子油纳米乳液冻干粉中,颗粒平均粒径121.3nm,藏红花酸包埋率90.3%,加热稳定性94%,储藏稳定性92%。
实施例5
1)栀子剥皮果在CO2流量25L/h,压力25MPa,温度50℃下进行超临界CO2萃取2h,得到栀子油;
2)将乳清分离蛋白溶于pH 7.0的0.1M磷酸盐缓冲溶液中,乳清分离蛋白与磷酸盐缓冲溶液料液比为1:10(质量/体积,g:mL),室温下搅拌6小时后,于4℃下冷藏保存,溶胀达12h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率150W,超声温度30℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(24000r/min,10min),将油相缓慢加入到水相中,形成初乳;
5)将制备好的初乳样品通过动态高压微射流纳米均质机(AH-1500,加拿大ATS公司),经过6次均质、均质压力为80MPa,得到单层栀子油纳米乳;
6)加入一定浓度的羧甲基纤维素钠溶液于单层栀子油纳米乳中,进行均质,经过6次均质、均质压力为90MPa,得到双层栀子油纳米乳,羧甲基纤维素钠在双层栀子油纳米乳中最终质量浓度为0.4g/100mL。
7)双层栀子油纳米乳,冷冻干燥48h,冷冻温度为-80℃,得到栀子油纳米乳液冻干粉。所得栀子油纳米乳液冻干粉中,颗粒平均粒径102.4nm,藏红花酸包埋率91.3%,加热稳定性94%,储藏稳定性95%。
实施例6
1)栀子剥皮果在CO2流量25L/h,压力25MPa,温度50℃下进行超临界CO2萃取2h,得到栀子油;
2)将大豆分离蛋白溶于pH 7.0的0.05M磷酸盐缓冲溶液中,大豆分离蛋白与磷酸盐缓冲溶液料液比为1:20(质量/体积,g:mL),室温下搅拌4小时后,于4℃下冷藏保存,溶胀达24h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率300W,超声温度40℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(28000r/min,10min),将油相缓慢加入到水相中,形成初乳;
5)将制备好的初乳样品通过动态高压微射流纳米均质机(AH-1500,加拿大ATS公司),经过3次均质、均质压力为50MPa,得到单层栀子油纳米乳;
6)加入一定浓度的羧甲基纤维素钠溶液于单层栀子油纳米乳中,进行均质,经过5次均质、均质压力为60MPa,得到双层栀子油纳米乳,羧甲基纤维素钠在双层栀子油纳米乳中最终质量浓度为0.4g/100mL。
7)双层栀子油纳米乳,冷冻干燥48h,冷冻温度为-80℃,得到栀子油纳米乳液冻干粉。所得栀子油纳米乳液冻干粉中,颗粒平均粒径121.3nm,藏红花酸包埋率90.2%,加热稳定性91%,储藏稳定性90.4%。
实施例7
1)栀子剥皮果在CO2流量35L/h,压力30MPa,温度60℃下进行超临界CO2萃取4h,得到栀子油;
2)将乳清分离蛋白溶于pH 7.0的0.1M磷酸盐缓冲溶液中,乳清分离蛋白与磷酸盐缓冲溶液料液比为1:16(质量/体积,g:mL),室温下搅拌4小时后,于4℃下冷藏保存,溶胀达12h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率200W,超声温度20℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(26000r/min,5min),将油相缓慢加入到水相中,形成初乳;
5)将制备好的初乳样品通过动态高压微射流纳米均质机(AH-1500,加拿大ATS公司),经过5次均质、均质压力为70MPa,得到单层栀子油纳米乳;
6)加入一定浓度的羧甲基纤维素钠溶液于单层栀子油纳米乳中,进行均质,经过6次均质、均质压力为90MPa,得到双层栀子油纳米乳,羧甲基纤维素钠在双层栀子油纳米乳中最终质量浓度为1.0g/100mL。
7)双层栀子油纳米乳,冷冻干燥48h,冷冻温度为-80℃,得到栀子油纳米乳液冻干粉。所得栀子油纳米乳液冻干粉中,颗粒平均粒径115.2nm,藏红花酸包埋率93%,加热稳定性94%,储藏稳定性92%。
实施例8
1)栀子剥皮果在CO2流量25L/h,压力25MPa,温度50℃下进行超临界CO2萃取2h,得到栀子油;
2)将乳清分离蛋白溶于pH 7.0的0.1M磷酸盐缓冲溶液中,乳清分离蛋白与磷酸盐缓冲溶液料液比为1:10(质量/体积,g:mL),室温下搅拌4小时后,于4℃下冷藏保存,溶胀达24h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率150W,超声温度30℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(24000r/min,10min),将油相缓慢加入到水相中,形成初乳;
5)将制备好的初乳样品通过动态高压微射流纳米均质机(AH-1500,加拿大ATS公司),经过6次均质、均质压力为90MPa,得到单层栀子油纳米乳;
6)加入一定浓度的羧甲基纤维素钠溶液于单层栀子油纳米乳中,进行均质,经过6次均质、均质压力为80MPa,得到双层栀子油纳米乳,羧甲基纤维素钠在双层栀子油纳米乳中最终质量浓度为0.4g/100mL。
7)双层栀子油纳米乳,冷冻干燥48h,冷冻温度为-80℃,得到栀子油纳米乳液冻干粉。所得栀子油纳米乳液冻干粉中,颗粒平均粒径121.7nm,藏红花酸包埋率81%,加热稳定性96%,储藏稳定性98%。
实施例1与实施例8对比可知,均质压力应当在适当范围内,在制备单层栀子油纳米乳的过程中,若均质压力过高反而导致了藏红花酸包埋率的下降,推测可能是由于均质压力较高导致了纳米乳形态的破坏。
实施例9
1)栀子剥皮果在CO2流量25L/h,压力25MPa,温度50℃下进行超临界CO2萃取2h,得到栀子油;
2)将乳清分离蛋白溶于pH 7.0的0.1M磷酸盐缓冲溶液中,乳清分离蛋白与磷酸盐缓冲溶液料液比为1:10(质量/体积,g:mL),室温下搅拌4小时后,于4℃下冷藏保存,溶胀达24h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率150W,超声温度30℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(24000r/min,10min),将油相缓慢加入到水相中,形成初乳;
5)将制备好的初乳样品通过动态高压微射流纳米均质机(AH-1500,加拿大ATS公司),经过6次均质、均质压力为50MPa,得到单层栀子油纳米乳;
6)加入一定浓度的羧甲基纤维素钠溶液于单层栀子油纳米乳中,进行均质,经过6次均质、均质压力为50MPa,得到双层栀子油纳米乳,羧甲基纤维素钠在双层栀子油纳米乳中最终质量浓度为0.6g/100mL。
7)双层栀子油纳米乳,冷冻干燥48h,冷冻温度为-80℃,得到栀子油纳米乳液冻干粉。所得栀子油纳米乳液冻干粉中,颗粒平均粒径136.7nm,藏红花酸包埋率91%,加热稳定性84%以上,储藏稳定性76%。
实施例1与实施例9对比可知,均质压力应当在适当范围内,在制备双层栀子油纳米乳的过程中,若均质压力过低,降低了加热稳定性和储藏稳定性,推测可能是由于均质压力较低导致了形成的双层纳米乳的结构不够稳定。
对比例1:单层栀子油纳米乳液冻干粉
1)栀子剥皮果在CO2流量25L/h,压力25MPa,温度50℃下进行超临界CO2萃取2h,得到栀子油;
2)将乳清分离蛋白溶于pH 7.0的0.1M磷酸盐缓冲溶液中,乳清分离蛋白与磷酸盐缓冲溶液料液比为1:10(质量/体积,g:mL),室温下搅拌4小时后,于4℃下冷藏保存,溶胀达24h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率150W,超声温度30℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(24000r/min,10min),将油相缓慢加入到水相中,形成初乳;
5)将制备好的初乳样品通过动态高压微射流纳米均质机(AH-1500,加拿大ATS公司),经过6次均质、均质压力为50MPa,得到单层栀子油纳米乳;
6)单层栀子油纳米乳,冷冻干燥48h,冷冻温度为-80℃,得到单层栀子油纳米乳液冻干粉。单层栀子油纳米乳液冻干粉中,颗粒平均粒径105nm,藏红花酸包埋率75%,加热稳定性65%,储藏稳定性达到54%。
对比例2:未冻干的双层栀子油纳米乳
1)栀子剥皮果在CO2流量25L/h,压力25MPa,温度50℃下进行超临界CO2萃取2h,得到栀子油;
2)将乳清分离蛋白溶于pH 7.0的0.1M磷酸盐缓冲溶液中,乳清分离蛋白与磷酸盐缓冲溶液料液比为1:10(质量/体积,g:mL),室温下搅拌4小时后,于4℃下冷藏保存,溶胀达24h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率150W,超声温度30℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(24000r/min,10min),将油相缓慢加入到水相中,形成初乳;
5)将制备好的初乳样品通过动态高压微射流纳米均质机(AH-1500,加拿大ATS公司),经过6次均质、均质压力为50MPa,得到单层栀子油纳米乳;
6)加入一定浓度的羧甲基纤维素钠溶液于单层栀子油纳米乳中,进行均质,经过6次均质、均质压力为80MPa,得到双层栀子油纳米乳,羧甲基纤维素钠在双层栀子油纳米乳中最终质量浓度为0.4g/100mL。
所得双层栀子油纳米乳中,颗粒平均粒径135.8nm,藏红花酸包埋率93%,加热稳定性68%,储藏稳定性63%。
对比例3:直接制备的双层栀子油纳米乳液冻干粉
1)栀子剥皮果在CO2流量25L/h,压力25MPa,温度50℃下进行超临界CO2萃取2h,得到栀子油;
2)将乳清分离蛋白溶于pH 7.0的0.1M磷酸盐缓冲溶液中,乳清分离蛋白与磷酸盐缓冲溶液料液比为1:10(质量/体积,g:mL),室温下搅拌4小时后,于4℃下冷藏保存,溶胀达24h,形成水相;
3)将50mg藏红花酸溶于100g栀子油中,超声处理30min(超声功率150W,超声温度30℃)至完全溶解,形成油相;
4)在高速分散机(D-500,北京大龙仪器有限公司)的作用下(24000r/min,10min),将油相缓慢加入到水相中,形成初乳;
5)加入一定浓度的羧甲基纤维素钠溶液于栀子油初乳中,在高速分散机(D-500,北京大龙仪器有限公司)的作用下(24000r/min,10min),得到双层栀子油纳米乳,羧甲基纤维素钠在双层栀子油纳米乳中最终质量浓度为0.4g/100mL;
6)双层栀子油纳米乳,冷冻干燥48h,冷冻温度为-80℃,得到栀子油纳米乳液冻干粉。所得栀子油纳米乳液冻干粉中,颗粒平均粒径201nm,藏红花酸包埋率61%,加热稳定性73%,储藏稳定性80%。
由实施例1与对比例1对比可知,单层栀子油纳米乳液冻干粉的藏红花酸包埋率、加热稳定性和储藏稳定性均远低于双层栀子油纳米乳冻干得到的栀子油纳米乳液冻干粉。说明本发明通过蛋白质、阴离子多糖的双层包埋,有效提高了包埋率和稳定性。
由实施例1与对比例2对比可知,若不经过冷冻干燥,加热稳定性和储藏稳定性都远远低于经过冷冻干燥的栀子油纳米乳液冻干粉,说明本发明经过冷冻干燥,能够长期留存有效成分,提高了稳定性和使用的方便性。
由实施例1与对比例3对比可知,若初乳不经过均质,直接由初乳形态加入多糖,高速分散制备双层栀子油纳米乳及冻干粉,其藏红花酸包埋率、加热稳定性和储藏稳定性都大幅降低,可见动态高压微射流技术能有效提高包埋率和稳定性。
本发明结合动态高压微射流技术和冷冻干燥技术,可明显提高藏红花酸的包埋率、纳米乳液颗粒的加热稳定性和储藏稳定性。
以上所述,仅为本发明较佳实施例而已,故不能依此限定本发明实施的范围,即依本发明专利范围及说明书内容所作的等效变化与修饰,皆应仍属本发明涵盖的范围内。
Claims (6)
1.一种栀子油纳米乳液冻干粉的制备方法,其特征在于:包括:
1)以蛋白的溶液作为水相,以添加了藏红花酸的栀子油作为油相,将油相加入到水相中,在24000~28000r/min分散5~10min,形成初乳;所述蛋白包括乳清分离蛋白或大豆分离蛋白中的至少一种;所述油相中,藏红花酸与栀子油的质量比为0.04~0.06:100;
2)将所述初乳通过动态高压微射流技术均质处理3~6次,均质压力为50~80MPa,得到单层栀子油纳米乳;
3)向所述单层栀子油纳米乳中加入阴离子多糖的溶液,通过动态高压微射流技术均质处理5~6次,均质压力为60~90MPa,得到双层栀子油纳米乳;所述阴离子多糖包括羧甲基纤维素钠或阿拉伯胶中的至少一种;
4)所述双层栀子油纳米乳在-85~-75℃冷冻干燥45~50h,得到所述栀子油纳米乳液冻干粉。
2.根据权利要求1所述的栀子油纳米乳液冻干粉的制备方法,其特征在于:所述步骤1)中,所述栀子油的制备方法包括:栀子剥皮果在CO2流量25~45L/h,压力10~35MPa,温度35~65℃下进行超临界CO2萃取0.5~6h,得到所述栀子油。
3.根据权利要求1所述的栀子油纳米乳液冻干粉的制备方法,其特征在于:所述步骤1)中,所述水相的制备方法包括:将蛋白按照1:20~1:10的料液比分散于pH 6.8~7.2的磷酸盐缓冲溶液中,室温下搅拌4~6小时后,0~5℃溶胀12~24h,得到所述水相。
4.根据权利要求1所述的栀子油纳米乳液冻干粉的制备方法,其特征在于:所述步骤1)中,所述油相的制备方法包括,采用超声处理20~30min至藏红花酸完全溶解于栀子油,超声处理的温度为20~40℃,超声功率为100~300W。
5.根据权利要求1所述的栀子油纳米乳液冻干粉的制备方法,其特征在于:所述步骤3)中,所述阴离子多糖在所述双层栀子油纳米乳中的最终质量浓度为0.4~1.0g/100mL。
6.一种根据权利要求1至5中任一项所述的制备方法所制备的栀子油纳米乳液冻干粉。
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