CN115336741A - 一种热处理协同3d打印制备抗消化淀粉的加工方法 - Google Patents
一种热处理协同3d打印制备抗消化淀粉的加工方法 Download PDFInfo
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Abstract
本发明属于食品加工领域,公开了一种热处理协同3D打印制备抗消化淀粉的加工方法。本发明选择脂质和多酚作为双配体,利用热处理协同3D打印诱导分子相互作用重排,构建一种具有高抗消化性能的V型结晶淀粉复合物,与此同时利用多酚抗氧化特性抑制热加工过程中脂质的氧化酸败,其抗消化淀粉含量可高达36.7%,同时氧化指标包括过氧化值、茴香胺值和总氧化值则分别降低至0.2,0.83和0.91。本发明所创制的抗消化淀粉具有制备方法简单,易于重复及批量生产等优势,适于食品领域产业化应用。
Description
技术领域
本发明属于食品加工技术领域,涉及一种热处理协同3D打印制备抗消化淀粉的加工方法。
背景技术
近年来随着与饮食相关的慢性代谢性疾病发病率逐年升高,营养健康膳食已成为现代食品科学及营养学领域的需求,现有学者研究发现食用抗消化淀粉(ResistantStarch,RS)可以有效调控人体血糖血脂代谢,降低肠道pH环境,提高肠道有益菌的丰度和数量,进而预防肥胖、糖尿病、心脑血管疾病和代谢综合症等营养失衡性疾病(Zheng B,Wang T,Wang H,et al.Studies on nutritional intervention of rice starch-oleicacid complex(resistant starch type V)in rats fed by high-fatdiet.Carbohydrate Polymers,2020,246)。其中,通过组分间相互作用(包括氢键、疏水作用力、范德华力和π-π共轭等)诱导淀粉与其他食品组分之间形成的复合物是一种新型抗消化淀粉,具有更高的营养价值。目前,由脂质配体通过疏水作用进入淀粉螺旋空腔内部,形成稳定具有抗酶解能力的淀粉脂质复合物,是常见的一种复合型抗消化淀粉(Krishnan V,Mondal D,Thomas B,et al.Starch-lipid interaction alters the molecularstructure and ultimate starch bioavailability:A comprehensivereview.International Journal of Biological Macromolecules,2021,182),其主要制备手段包括蒸汽喷射蒸煮法、螺杆挤出法、湿热法等。虽然以上热加工方法能较普通的蒸煮法提高制备效率,但过程中往往伴随着强烈的机械剪切和热效应,容易导致不饱和脂质氧化酸败,进而产生“哈喇”味和一些小分子有害物质的产生,降低了复合物的风味和营养特性,因此调控复合物消化性能的同时也需关注加工过程中脂质氧化酸败问题,以保证其更高的营养功能。多酚类物质作为植源性活性成分,具有如降血压、抗癌等多种营养功能,逐渐被用于食品加工中来丰富食品的营养品质。研究显示多酚具有较好抗氧化功能,其可通过π-π共轭竞争性地与不饱和脂肪酸争夺活性氧,同时结合脂质氧化自由基,使自由基转化为惰性化合物,进而终止脂质氧化链式反应(Lv Q,Long J,Gong Z,et al.Current Stateof Knowledge on the Antioxidant Effects and Mechanisms of Action ofPolyphenolic Compounds.Natural Product Communications,2021,16)。同时,多酚中亦可通过疏水作用进入淀粉螺旋空腔构成V型复合物,并通过分子间氢键作用促使分子链有序重排,提高淀粉有序化程度,进而有效提高淀粉的抗消化性能(Deng N,Deng Z,Tang C,et al.Formation,structure and properties of the starch-polyphenol inclusioncomplex:A review.Trends in Food Science&Technology,2021,112)。因此,可在淀粉与脂质体系中适当添加多酚分子,在防止脂质氧化的同时赋予体系更高的抗消化性能,具有很好的实际价值。目前,对于脂质与多酚同时诱导淀粉构建复合抗消化淀粉的研究暂未见报道。
由此可见,有必要研究一种在提高淀粉抗消化性能的同时抑制加工过程中脂质氧化酸败的加工方法,创制出健康安全的抗消化淀粉。
发明内容
本发明的首要目的是提供一种热处理协同3D打印制备抗消化淀粉的加工方法。本发明通过热处理首先对淀粉-脂质-多酚三元复合物进行预处理,进一步协同低温3D打印技术制备三元抗消化淀粉,在提高淀粉抗消化性能的同时抑制加工过程中脂质的氧化酸败,进而创制出健康安全的抗消化淀粉。
本发明另一目的在于提供上述方法制备的抗消化淀粉。
实现本发明目的的具体技术方案是:
一种热处理协同3D打印制备抗消化淀粉的加工方法,包括以下步骤:
(1)三元混合物的热处理:将脂质、多酚和淀粉混合均匀后置于油浴锅中进行热处理,获得热处理三元混合物;
(2)打印基料的制备:将热处理三元混合物置于盛有一定量的蒸馏水三口烧瓶中,后水浴加热使其凝胶化,同时在数显电动机搅拌下制备成均匀的打印基料
(3)利用3D打印低温制备抗消化淀粉:将制备好的打印基料装填至打印机料筒中进行保温,后利用食品热挤压3D打印机进行打印制备抗消化淀粉。
优选的,步骤(1)所述淀粉为大米淀粉或小麦淀粉,所述脂质为玉米油、橄榄油、油酸或亚油酸,所述多酚为白藜芦醇、咖啡酸或绿原酸;
优选的,步骤(1)所述脂质、多酚和淀粉混合是按质量份数计,将0.3-3.0份脂质,0-1.8份多酚溶于5份无水乙醇中,后缓慢均匀喷洒至30份淀粉中,同时边喷洒边搅拌使其分散均匀;
优选的,步骤(1)所述热处理前需将油浴预热至热处理温度90-130℃,同时在热处理过程不断搅拌以保证混合物受热均匀,热处理时间为1-3h;
优选的,步骤(2)所述打印基料的浓度是按质量份数计,将20-30份热处理三元混合物置于盛有100份蒸馏水的三口烧瓶中;
优选的,步骤(2)所述水浴加热是指在打印基料制备前将水浴锅预热至凝胶化温度40-60℃,在此温度条件下水浴加热15-30min;所述搅拌是指不断旋转搅拌以保证基料受热均匀,其中搅拌桨转速为100-180r/min;
优选的,步骤(3)所述3D打印低温制备是采用食品热挤压3D打印机,打印前料筒提前预热至设定打印温度35-55℃并保温1-5min;
优选的,步骤(3)所述3D打印低温制备,其打印参数为喷嘴高度0.7mm,喷嘴直径0.4-1.0mm,打印速度60mm/s,回抽速度60mm/s,回抽距离1.8mm。
一种由上述方法制备的抗消化淀粉。
本发明的发明机理:
干热处理作为常用的食品加工方法,操作简单,其能够通过热能破坏淀粉颗粒结构,使内部分子链部分发生断裂,并在水分子迁移过程中诱导淀粉分子有序重排及与其他组分间相互作用构建有序结构;而热挤压3D打印通过喷嘴剪切和层层沉积诱导分子相互作用重排,形成致密有序的空间结构,同时赋予其个性化外观。本专利构建一种热处理协同3D打印制备抗消化淀粉的加工方法,该加工方法利用干热预处理破坏淀粉原有的颗粒结构,并促进淀粉与脂质和多酚的相互作用,在此基础上通过低温3D打印增强组分间的相互作用,进一步提高内部的有序结构,进而提高淀粉复合物的抗消化性能。同时,基于淀粉-脂质-多酚之间的相互作用还可以抑制加工过程中脂质的氧化酸败,进而创制出健康安全的抗消化淀粉。
与现有技术相比,本发明具有以下优点及有益效果:
(1)本发明通过热处理协同低温3D打印技术制备抗消化淀粉,相较于传统的淀粉-脂质复合物制备,淀粉-脂质-多酚三元复合物具有更好的抗消化性能和抗氧化特性,其抗消化性能RS和SDS分别高达36.7%和9.2%,其氧化指标包括过氧化值、茴香胺值和总氧化值则分别降低至0.2,0.83和0.91。
(2)本发明利用脂质和多酚作为双重配位体,构建新型的三元淀粉复合物,相较于传统的淀粉-脂质复合物制备,多酚的引入可以通过π-π共轭争夺活性氧,同时结合脂质氧化自由基转化为惰性化合物,进而终止脂质氧化酸败的链式反应,降低复合物的过氧化值、茴香胺值和总氧化值,进而提高淀粉复合物的安全性。
(3)本发明通过热处理协同低温3D打印技术制备抗消化淀粉,其中热处理使得淀粉颗粒破裂,分子链发生部分断裂,此时脂质和多酚在热效应作用下,尤其是脂质,渗透进入淀粉颗粒内部,与分子链相互作用形成部分复合物;而低温3D打印主要利用水分子的迁移行为破坏淀粉颗粒的无定形区域,而较好地保留淀粉原有的有序化结构,且释放的分子链在3D打印剪切和沉积的诱导作用下与体系中脂质和多酚发生分子互作,形成有序的“V”型结晶结构,进而提高淀粉的抗消化能力。
(4)本发明所创制的抗消化淀粉具有制备方法简单,易于重复及批量生产等优势,且营养功能更为丰富,适于食品领域产业化应用。
附图说明
图1为原大米淀粉、热处理后实施例1、6和对比例1、2的SEM图。
图2为原大米淀粉、热处理协同3D打印制备的实施例1、6和对比例1、2的XRD图。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。本发明涉及的所使用的材料、试剂、设备等,如无特殊说明,均可从市场上直接购买。
实施例1
步骤1:按质量份数计,将2.4份油酸、0.3份绿原酸和30份大米淀粉混合均匀后置于油浴锅中在120℃温度条件下进行热处理120min,获得热处理三元混合物;
步骤2:按质量份数计,将25份的热处理三元混合物置于盛有100份蒸馏水三口烧瓶中,在50℃条件下水浴加热20min使其凝胶化,在数显电动机搅拌下制备成均匀的打印基料,转速为120r/min;
步骤3:将制备好的混合物打印基料装填至打印机料筒中在50℃温度下保温5min,利用食品热挤压3D打印机进行打印制备抗消化淀粉(抗消化淀粉1),打印参数为喷嘴高度0.7mm,喷嘴直径0.6mm,打印速度60mm/s,回抽速度60mm/s,回抽距离1.8mm;
实施例2
本实施例与实施例1的区别在于,步骤1中大米淀粉替换为小麦淀粉,制备抗消化淀粉(抗消化淀粉2)。
实施例3
本实施例与实施例1的区别在于,步骤1中油酸替换为玉米油,制备抗消化淀粉(抗消化淀粉3)。
实施例4
本实施例与实施例1的区别在于,步骤1中绿原酸替换为白藜芦醇,制备抗消化淀粉(抗消化淀粉4)。
实施例5
本实施例与实施例1的区别在于,步骤1中油酸添加量由2.4份替换为0.6份,制备抗消化淀粉(抗消化淀粉5)。
实施例6
本实施例与实施例1的区别在于,步骤1中绿原酸添加量由0.3替换为1.5份,制备抗消化淀粉(抗消化淀粉6)。
实施例7
本实施例与实施例1的区别在于,步骤1中热处理温度由120℃替换为130℃,制备抗消化淀粉(抗消化淀粉7)。
实施例8
本实施例与实施例1的区别在于,步骤1中热处理时间由2h替换为3h,制备抗消化淀粉(抗消化淀粉8)。
实施例9
本实施例与实施例1的区别在于,步骤2中水浴温度由50℃替换为60℃,制备抗消化淀粉(抗消化淀粉9)。
实施例10
本实施例与实施例1的区别在于,步骤2中混合物含量由25份替换为20份,制备抗消化淀粉(抗消化淀粉10)。
实施例11
本实施例与实施例1的区别在于,步骤2中转速由120r/min替换为180r/min,制备抗消化淀粉(抗消化淀粉11)。
实施例12
本实施例与实施例1的区别在于,步骤3中打印温度由50℃替换为40℃,制备抗消化淀粉(抗消化淀粉12)。
实施例13
本实施例与实施例1的区别在于,步骤3中喷嘴直径由0.6mm换为1.0mm,制备抗消化淀粉(抗消化淀粉13)。
对比例1
(1)按质量份数计,将30份大米淀粉置于油浴锅中在120℃温度条件下进行热处理120min,获得热处理大米淀粉;(2)将25份的热处理大米淀粉置于盛有100份蒸馏水三口烧瓶中,在50℃条件下水浴加热20min使其凝胶化,在数显电动机搅拌下制备成均匀的打印基料,转速为120r/min;(3)将制备好的基料置于打印机料筒中在50℃温度下保温5min,利用食品热挤压3D打印机进行打印制备,打印参数为喷嘴高度0.7mm,喷嘴直径0.6mm,打印速度60mm/s,回抽速度60mm/s,回抽距离1.8mm;
对比例2
(1)按质量份数计,将2.4份油酸和30份大米淀粉混合均匀后置于油浴锅中在120℃温度条件下进行热处理处理120min,获得热处理二元混合物;(2)将25份的热处理混合物置于盛有100份蒸馏水三口烧瓶中,在50℃条件下水浴加热20min使其凝胶化,在数显电动机搅拌下制备成均匀的打印基料,转速为120r/min;(3)将制备好的基料置于打印机料筒中在50℃温度下保温5min,利用食品热挤压3D打印机进行打印制备抗消化淀粉,打印参数为喷嘴高度0.7mm,喷嘴直径0.6mm,打印速度60mm/s,回抽速度60mm/s,回抽距离1.8mm;
对比例3
本对比例与对比例2的区别在于,步骤1中的油酸替代为玉米油;
对比例4
(1)按质量份数计,将2.4份油酸、0.3份绿原酸和30份大米淀粉混合均匀后置于油浴锅中在120℃温度条件下进行热处理120min,获得热处理三元混合物;(2)将25份的热处理混合物置于盛有100份蒸馏水打印料筒中,利用食品热挤压3D打印机进行打印制备抗消化淀粉,打印参数为喷嘴高度0.7mm,喷嘴直径0.6mm,打印速度60mm/s,回抽速度60mm/s,回抽距离1.8mm;
对比例5
(1)按质量份数计,将2.4份油酸、0.3份绿原酸和30份大米淀粉混合均匀后置于油浴锅中在120℃温度条件下进行热处理120min,获得热处理三元混合物;(2)将25份的热处理混合物置于盛有100份蒸馏水三口烧瓶中,在高温95℃条件下水浴加热使其凝胶化,在数显电动机搅拌下制备成均匀的打印基料;(3)将制备好的基料置于打印机料筒中在70℃温度下保温5min,利用食品热挤压3D打印机进行打印制备抗消化淀粉,打印参数为喷嘴高度0.7mm,喷嘴直径0.6mm,打印速度60mm/s,回抽速度60mm/s,回抽距离1.8mm;
对比例6
(1)按质量份数计,将2.4份油酸、0.3份绿原酸和30份大米淀粉混合均匀后置于油浴锅中在120℃温度条件下进行热处理120min,获得热处理三元混合物;(2)将25份的热处理混合物置于盛有100份蒸馏水三口烧瓶中,在50℃条件下水浴加热20min使其凝胶化,在数显电动机搅拌下制备成均匀的打印基料,转速为120r/min;(3)将制备好的基料置于打印机料筒中在70℃温度下保温5min,利用食品热挤压3D打印机进行打印制备抗消化淀粉,打印参数为喷嘴高度0.7mm,喷嘴直径0.6mm,打印速度60mm/s,回抽速度60mm/s,回抽距离1.8mm;
本发明对上述实施例利用SEM以及XRD进行表征,并对实施例和对比例制得的抗消化淀粉的消化性能和氧化指标进行测定,具体如下:
(1)颗粒形貌
将热处理后的淀粉及其淀粉复合物颗粒涂抹至粘有导电双面胶的样品台中上,用洗耳球将多余的颗粒吹走保证颗粒处于同一聚焦水平;将样品台置于离子溅射镀膜仪中镀金5min,然后在20kV电压下选择4.0×103放大倍数进行观察拍照。
(2)结晶结构
将热处理协同3D打印制备的的淀粉及其淀粉复合物进行冷冻干燥后粉碎筛分(200目);将筛分后的样品粉末压紧后置于XRD样品台中,采用波长为0.1542nm的单色Cu-Kα射线,在管压40kV,管流40mA条件下选择步长0.0165°进行连续扫描,扫描范围为5-40°。
(3)氧化指标测试
本发明中实施例的氧化特性指标的测定方法参照国标GB 5009.227-2016和GB/T24304-2009,包括其过氧化值、茴香胺值和总氧化值。
(4)消化性能测试
本发明中实施例的消化性质的测定方法为:采用Sigma公司的酶(猪胰α-淀粉酶:P-7545和淀粉葡萄糖苷酶:A-3360),参考Englyst提出的步骤分析其快消化淀粉(RDS)、慢消化淀粉(SDS)和抗消化淀粉(RS)的含量。
测定结果:
图1为原大米淀粉、热处理后实施例1、6和对比例1、2的SEM图,由图可知淀粉经过热处理后颗粒表面变得凹凸不平,这是由于在热处理过程中淀粉中水分迁移,无定形区融胀破坏,导致其外观形貌发生不规则变化;随着脂质和多酚的添加,其外观形貌不规则度增加,同时伴随着大量坑洼的出现,说明脂质多酚在热能作用下向淀粉无定形区域进行迁移并与淀粉发生复合进行导致原有的颗粒形貌破坏。
图2为原大米淀粉、热处理协同3D打印后实施例1、6和对比例1、2的XRD图,由图可知原大米淀粉经过加工处理后,其原有的A型结晶特征峰消失,同时未有其他新的特征峰形成,呈现一个较大的弥散峰;伴随着脂质多酚的添加,淀粉分子链与脂质多酚发生疏水复合,形成有序的V型结晶结构,于13.6°和20.1°处出现明显的结晶特征峰。随着脂质多酚添加量的增加,其结晶特征峰愈发明显,表明样品结晶度有所增加。
表1为不同实施例及对比例的氧化指标和消化性能。由表可知,相较于对比例1-3可知,实施例的氧化指标均明显降低,其抗消化性能显著增加,其中实施例6的抗消化淀粉RS高达36.7%,其氧化指标包括过氧化值、茴香胺值和总氧化值则分别降低至0.2,0.83和0.91。对比实施例4-6发现,当热处理三元复合物未经过凝胶化时,其淀粉保持颗粒状态不能成功形成凝胶网结构,导致3D打印失败;而当其凝胶化温度或打印温度过高,淀粉处于完全糊化状态时,伴随着脂质氧化加剧和原有有序结构崩解,导致其氧化指标和抗消化能力下降。由实施例2可知,在热加工过程中,大米淀粉相较于小麦淀粉其复合能力相对较强,这是由于大米淀粉颗粒较小,在加工过程中其可以更好地与脂质多酚互作,进而提高淀粉抗消化能力。由实施例3可知,在热加工过程中,油酸相较于玉米油更容易发生氧化酸败,但其复合能力相对较强,可提高淀粉抗消化能力。由实施例4可知,白藜芦醇的抗氧化能力和复合能力相较于绿原酸较弱。由实施例5可知,随着油酸添加量的增加,其抗消化性能有所增加,但同时伴随着更剧烈的氧化酸败。由实施例6-8,10,11可知,随着加工过程中温度升高,加热处理时间变长,搅拌转速增加,脂质将与氧气接触更加充分,进而发生更严重的氧化,同时淀粉原有的有序结构被进一步破坏,导致其抗消化性能有所降低。由实施例10,13可知,随着打印基料浓度增加,喷嘴直径降低,3D打印过程中的剪切诱导淀粉脂质多酚分子互作重排效果更加明显,形成的复合物抗消化能力更强。
由以上实施例和对比例结果可知,淀粉和淀粉脂质复合物经过热处理和3D打印处理存在抗消化性能低、氧化酸败严重的缺点;由于多酚的添加,淀粉-脂质-多酚三元体系复合物抗消化性能显著增加,同时多酚对脂质的氧化酸败起到了明显的抑制作用。相较于传统的淀粉脂质复合物,三元淀粉复合物氧化酸败程度更低,抗消化性能更佳。
表1实施例及对比例的氧化指标和消化性能
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明,不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的技术人员来说,在不脱离本发明构思的前提下,还可以做出若干等同替代或明显变型,而且性能或用途相同,都应当视为属于本发明的保护范围。
Claims (9)
1.一种热处理协同3D打印制备抗消化淀粉的加工方法,其特征在于,包括以下步骤:
(1)三元混合物的热处理:将脂质、多酚和淀粉混合均匀后置于油浴锅中进行热处理,获得热处理三元混合物;
(2)打印基料的制备:将热处理三元混合物置于盛有一定量的蒸馏水三口烧瓶中,后水浴加热使其凝胶化,同时在数显电动机搅拌下制备成均匀的打印基料;
(3)利用3D打印低温制备抗消化淀粉:将制备好的打印基料装填至打印机料筒中进行保温,后利用食品热挤压3D打印机进行打印制备抗消化淀粉。
2.根据权利要求1所述的制备方法,其特征在于:步骤(1)所述淀粉为大米淀粉或小麦淀粉,所述脂质为玉米油、橄榄油、油酸或亚油酸,所述多酚为白藜芦醇、咖啡酸或绿原酸。
3.根据权利要求1所述的制备方法,其特征在于:步骤(1)所述脂质、多酚和淀粉混合是按质量份数计,将0.6-2.4份脂质,0.3-1.5份多酚溶于5份无水乙醇中,后缓慢均匀喷洒至30份淀粉中,同时边喷洒边搅拌使其分散均匀。
4.根据权利要求1所述的制备方法,其特征在于:步骤(1)所述热处理前需将油浴预热至热处理温度90-130℃,同时在热处理过程不断旋转搅拌以保证混合物受热均匀,热处理时间为1-3h。
5.根据权利要求1所述的制备方法,其特征在于:步骤(2)所述打印基料浓度是按质量份数计,将20-30份热处理三元混合物置于盛有100份蒸馏水的三口烧瓶中。
6.根据权利要求1所述的制备方法,其特征在于:步骤(2)所述打印基料制备前将水浴锅预热至凝胶化温度40-60℃,在此温度条件下水浴加热15-30min;所述搅拌是不断旋转搅拌以保证基料受热均匀,其中搅拌桨转速为100-180r/min。
7.根据权利要求1所述的制备方法,其特征在于:步骤(3)所述打印制备采用食品热挤压3D打印机,打印前料筒提前预热至设定打印温度35-55℃并保温1-5min。
8.根据权利要求1所述的制备方法,其特征在于:步骤(3)所述3D打印低温制备,其打印参数为喷嘴高度0.7mm,喷嘴直径0.4-1.0mm,打印速度60mm/s,回抽速度60mm/s,回抽距离1.8mm。
9.一种由权利要求1~8任一项所述方法制备的抗消化淀粉。
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