CN114052159A - 一种包埋香气物质的缓释凝胶及其制备方法和应用 - Google Patents
一种包埋香气物质的缓释凝胶及其制备方法和应用 Download PDFInfo
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- CN114052159A CN114052159A CN202111473543.1A CN202111473543A CN114052159A CN 114052159 A CN114052159 A CN 114052159A CN 202111473543 A CN202111473543 A CN 202111473543A CN 114052159 A CN114052159 A CN 114052159A
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- gel
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- aroma substances
- pectin
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- Jellies, Jams, And Syrups (AREA)
Abstract
本发明涉及食品加工技术领域,具体提供了一种包埋香气物质的缓释凝胶及其制备方法和应用,该包埋香气物质的缓释凝胶的制备方法包括如下步骤:将果胶与盐溶液混合,得到第一混合液,将第一混合液与香气物质混合,调节pH值为1‑3,在温度为60‑100℃下静置,离心,获得凝胶,该凝胶可以笼络挥发性香气物质,实现挥发性香气物质的高效包埋。凝胶结构的稳定性可以避免加工过程中香气物质的损失,提高香气物质的保留率,加入果蔬制品中可以缓慢释放香气物质,并且在果胶裂解酶等的作用下实现释放速率可调节。
Description
技术领域
本发明涉及食品加工技术领域,具体涉及一种包埋香气物质的缓释凝胶及其制备方法和应用。
背景技术
果蔬榨汁得到的果蔬汁悬浮物,包括果肉、皮碎屑和一些不溶于水的大颗粒成分组成了一个混浊的具有稳定的胶体系统,因其含有果肉碎块以及溶入果蔬汁中的蛋白质、酚类物质、果胶、阿拉伯聚糖、淀粉、右旋糖酐等容易引起混浊,现有工艺通常直接采用渣汁分离式榨汁机或者榨汁后再离心的方式去除果汁中的悬浮大颗粒,还可以通过胶体磨、均质等方法将悬浮大颗粒微粒化处理以提高果汁品质,延长存储时间。然而在这些加工过程中不同程度的普遍存在香气损失或逸散等问题,严重影响产品品质,降低消费者的购买欲望。
现有技术中通过直接添加香精香料的方式来增加香气,但是,果蔬汁中的香气是由多种呈香的挥发性物质所组成(如萜类、醇类、酯类、醛类和酮类等小分子化合物),这些物质在加工过程中,易降解、易损失,无法实现产品货架期的持久释放。
发明内容
因此,本发明的目的在于提供一种包埋香气物质的缓释凝胶制备方法及应用。
本发明提供了一种包埋香气物质的缓释凝胶的制备方法,其特征在于,包括如下步骤:
S1步骤:将果胶与盐溶液混合,得到第一混合液;
S2步骤:将第一混合液与香气物质混合,调节pH值为1-3,在温度为60-100℃下静置,离心,获得凝胶。
进一步地,所述果胶的质量与盐溶液的体积比为0.1-7:100。其中质量与体积的比值关系为g/mL。其中,优选为3-7:100。
进一步地,所述果胶与香气物质的质量比为104-108:1。
进一步地,所述盐溶液选自氯化钠水溶液和/或柠檬酸钠水溶液。
进一步地,所述盐溶液的浓度为0.05-20wt%。
进一步地,所述香气物质选自柠檬烯、巴伦西亚橘烯、水芹烯、月桂烯、蒎烯、桧烯、罗勒烯、萜品油烯、松油烯、榄香烯、石竹烯、壬醛和乙酸乙酯中的至少一种。
进一步地,S2步骤中,采用常规的酸试剂调节pH值,例如柠檬酸、苹果酸等。优选采用质量为5-20g/L的酸试剂。
进一步地,S1步骤和/或S2步骤中,在200-3000rpm的搅拌下进行混合,混合时间为5-60min。
进一步地,S2步骤中,静置时间至少为5min,优选为5-30min。
进一步地,S2步骤中,混合之前还包括将第一混合液的pH值调为5-7,然后在温度为20-35℃的条件下与果胶甲酯酶反应的步骤。具体地可采用NaOH、KOH等碱性物质的水溶液调节pH值,碱性物质的水溶液的浓度为5-10wt%。
优选地,采用果胶甲酯酶水溶液与第一混合液进行反应,果胶甲酯酶水溶液的浓度为2-50U/mL,加入果胶甲酯酶体积为果胶溶液体积的1/100-1/10。
进一步地,离心步骤之前还包括加入金属盐溶液混合后再静置的步骤。
进一步地,金属盐溶液及质量浓度为包括但不限于海藻酸钠1-3.5%,氯化钙2-3%,硬脂酰乳酸钠0.2-0.5%中的一种或几种。
进一步地,添加金属盐溶液后混合的温度和pH条件为:20-35℃,pH为4-7。添加金属盐溶液后混合时间为5-60min。添加金属盐溶液后静置时间:5-60min。
进一步地,S2步骤之后还包括对凝胶进行干燥获得香气物质粉制剂的步骤。优选采用冷冻干燥。
本发明还提供了上述任一所述的包埋香气物质的缓释凝胶制备方法制得的凝胶或者由所述的凝胶干燥后得到的凝胶粉在食品中的应用。
本发明还提供了一种食品,包括本发明任一所述的凝胶或者凝胶粉。优选地所述食品选自饮料或者果酱,饮料选自果蔬汁饮料、茶饮料或者乳饮料,果蔬汁饮料包括果汁、蔬菜汁、蔬果汁等,果汁可以是橙子、苹果汁、百香果汁、火龙果汁、葡萄汁等,茶饮料选自乌龙茶、绿茶、红茶等,乳饮料选自牛奶、酸奶、奶茶等。
本发明中的果汁的制备方法包括如下步骤,榨汁-加入凝胶混料-胶体磨研磨-均质-灭菌。
进一步,每升果汁加入0.1-500g凝胶,优选地,每升果汁加入1-10g凝胶。
进一步,还包括果胶裂解酶,优选地,果胶裂解酶的添加量为10-5000U/100g凝胶,更优选地,果胶裂解酶的添加量为1000-3000U/100g凝胶。
进一步,在温度为2-6℃,压力为18-22MPa下进行均质处理。
进一步,采用超高压灭菌,控制压力为580-620MPa,时间为4-6min。
本发明技术方案,具有如下优点:
1.本发明提供的包埋香气物质的缓释凝胶的制备方法,研究发现将果胶与盐溶液混合,再与香气物质混合,调节pH值为1-3,在温度为60-100℃下静置,离心,可获得凝胶结构网络,这种凝胶网络结构的空腔区域可以笼络挥发性香气物质,实现挥发性香气物质的高效包埋。凝胶结构的稳定性可以避免加工过程中香气物质的损失,提高香气物质的保留率,加入果汁等食品中可以缓慢释放香气物质,并且在果胶裂解酶等的作用下实现释放速率可调节。
2.本发明提供的包埋香气物质的缓释凝胶的制备方法,通过控制所述果胶的质量与盐溶液的体积比为0.1-7:100,或者控制所述果胶与香气物质的质量比为104-108:1,能够进一步提高香气物质的保留率。
3.本发明提供的食品,凝胶形成的高强度的凝胶网络在改善果蔬汁汁挥发性香气的基础上,可以进一步提高食品的粘度,以果汁为例,可以增强果汁的混浊稳定性,延缓果汁储藏期间的沉淀分层现象。
具体实施方式
提供下述实施例是为了更好地进一步理解本发明,并不局限于所述最佳实施方式,不对本发明的内容和保护范围构成限制,任何人在本发明的启示下或是将本发明与其他现有技术的特征进行组合而得出的任何与本发明相同或相近似的产品,均落在本发明的保护范围之内。
实施例中未注明具体实验步骤或条件者,按照本领域内的文献所描述的常规实验步骤的操作或条件即可进行。所用试剂或仪器未注明生产厂商者,均为可以通过市购获得的常规试剂产品。
本发明的果胶可以来自市购,例如购自麦克林生化科技有限公司,型号P885045,也可以采用植物源果胶,例如采用水果蔬菜冷冻后用无水乙醇破碎,过滤,烘干后制得,所用水果蔬菜可以但不限于苹果、柑橘、山楂、柿子、石榴、鲜枣、梨、香蕉、花椰菜、马铃薯、百香果、火龙果、葡萄等。
本发明各实施例和对比例采用的果胶由如下方法制得:将100g橙汁用液氮冷冻,在500mL无水乙醇中破碎混匀,过滤后得到的滤渣在无水乙醇中重复提取两次,最后得到的滤渣40℃烘干20h得到果胶粉末。
果胶裂解酶购自夏盛生物科技有效公司,型号FDY-2211。果胶甲酯酶购自西格玛奥德里奇(上海)贸易有限公司,型号P5400。
实施例1
本实施例提供了一种包埋香气物质的缓释凝胶的制备方法,包括如下步骤:
S1步骤:取7g果胶加入到100mL质量百分数为20%的NaCl溶液,在200rpm下搅拌10min,得到第一混合液;
S2步骤:将第一混合液与1μg柠檬烯混合,在200rpm下搅拌10min,加入10g/L的柠檬酸水溶液调节混合液的pH值为2.0,在温度为85℃下静置10min,离心(转速为10000rpm,时间为10min),去除上清液,收集下层凝胶。
本实施例还提供了一种橙汁,其制备方法包括如下步骤:
将橙子肉采用渣汁分离式榨汁机(九阳股份有限公司JYZ-E3)榨汁,得到纯橙汁,取500mL纯橙汁加入按照本实施例方法制得的凝胶2g混合,经胶体磨研磨后,置于均质机中,在温度为4℃,压力为20MPa下进行均质处理,然后进行超高压灭菌,压力600Mpa,时间为5min,即得橙汁。
实施例2
本实施例提供了一种包埋香气物质的缓释凝胶的制备方法,包括如下步骤:
S1步骤:取10g果胶加入到300mL质量百分数为0.05%的柠檬酸钠溶液混合,在300rpm下搅拌10min,得到第一混合液;
S2步骤:将第一混合液与5μg柠檬烯混合,在300rpm下搅拌30min,加入10g/L的柠檬酸水溶液调节混合液的pH值为3.0,在温度为100℃下静置30min,离心(转速为8000rpm,时间为10min),去除上清液,收集下层凝胶。
本实施例还提供了一种橙汁,其制备方法包括如下步骤:
将橙子肉采用渣汁分离式榨汁机(九阳股份有限公司JYZ-E3)榨汁,得到纯橙汁,取500mL纯橙汁加入按照本实施例方法制得的凝胶2g和20U果胶裂解酶混合,经胶体磨研磨后,置于均质机中,在温度为4℃,压力为20MPa下进行均质处理,然后进行超高压灭菌,压力600MPa,时间为5min,即得橙汁。
实施例3
本实施例提供了一种包埋香气物质的缓释凝胶的制备方法,包括如下步骤:
S1步骤:取6g果胶与1wt%NaCl溶液100mL混合,在300rpm下搅拌10min,得到第一混合液;
S2步骤:将第一混合液与0.3μg月桂烯混合,在300rpm下搅拌30min,加入5g/L的柠檬酸水溶液调节混合液的pH值为1.0,在温度为60℃下静置30min,离心(转速为4000rpm,时间为5min),去除上清液,收集下层凝胶。
本实施例还提供了一种橙汁,其制备方法包括如下步骤:
将橙子肉采用渣汁分离式榨汁机(九阳股份有限公司JYZ-E3)榨汁,得到纯橙汁,取500mL纯橙汁加入按照本实施例方法制得的凝胶2g混合,经胶体磨研磨后,置于均质机中,在温度为4℃,压力为20MPa下进行均质处理,然后进行超高压灭菌,压力600MPa,时间为5min,即得橙汁。
实施例4
本实施例提供了一种包埋香气物质的缓释凝胶的制备方法,包括如下步骤:
S1步骤:取6g果胶加入到100mL质量百分数为1%的NaCl溶液中,在300rpm下搅拌10min,得到第一混合液;
S2步骤:用5wt%的NaOH水溶液将第一混合液的pH值调节为7.0,在25℃下加入50U/mL果胶甲酯酶水溶液2mL,25℃下反应20min后再与0.3g月桂烯混合,在300rpm下搅拌30min,加入10g/L的柠檬酸水溶液调节混合液的pH值为1.0,在温度为60℃下静置30min,离心(转速为3000rpm,时间为15min),去除上清液,收集下层凝胶。
本实施例还提供了一种梨汁,其制备方法包括如下步骤:
将梨肉采用渣汁分离式榨汁机(九阳股份有限公司JYZ-E3)榨汁,得到纯梨汁,取500mL纯梨汁加入按照本实施例方法制得的凝胶20g混合,经胶体磨研磨后,置于均质机中,在温度为4℃,压力为20MPa下进行均质处理,然后进行超高压灭菌,压力580MPa,时间为6min,即得梨汁。
实施例5
本实施例提供了一种包埋香气物质的缓释凝胶的制备方法,包括如下步骤:
S1步骤:取6g果胶加入到100mL质量百分数为1%的NaCl溶液中,在300rpm下搅拌10min,得到第一混合液;
S2步骤:将第一混合液与0.3μg月桂烯混合,在300rpm下搅拌30min,加入5g/L的苹果酸水溶液调节混合液的pH值为1.0,在温度为60℃下静置30min,加入2wt%氯化钙溶液20mL,在300rpm下搅拌10min,静置20min,离心(转速为2000rpm,时间为30min),去除上清液,收集下层凝胶。
本实施例还提供了一种橙汁,其制备方法包括如下步骤:
将橙子肉采用渣汁分离式榨汁机(九阳股份有限公司JYZ-E3)榨汁,得到纯橙汁,取500mL纯橙汁加入按照本实施例方法制得的凝胶200g混合,经胶体磨研磨后,置于均质机中,在温度为4℃,压力为20MPa下进行均质处理,然后进行超高压灭菌,压力600MPa,时间为5min,即得橙汁。
对比例1
本对比例提供了一种包埋香气物质的缓释凝胶的制备方法,包括如下步骤:
S1步骤:取7g果胶加入到100mL质量百分数为20%的NaCl溶液,加入1g柠檬烯,在200rpm下搅拌20min,离心(转速为5000rpm,时间为10min),去除上清液,收集下层凝胶。
本对比例还提供了一种橙汁,其制备方法与实施例1基本相同,区别仅在于加入的凝胶采用本对比例的方法制得。
对比例2
本对比例提供了一种包埋香气物质的缓释凝胶的制备方法,与实施例1基本相同,区别仅在于S2步骤采用10g/L的柠檬酸水溶液调节混合液的pH值为4.5。
本对比例还提供了一种橙汁,其制备方法与实施例1基本相同,区别仅在于加入的凝胶采用本对比例的方法制得。
对比例3
本对比例提供了一种包埋香气物质的缓释凝胶的制备方法,与实施例1基本相同,区别仅在于S2步骤调节pH值为2.0后,在温度为40℃下静置10min。
本对比例还提供了一种橙汁,其制备方法与实施例1基本相同,区别仅在于加入的凝胶采用本对比例的方法制得。
实验例1
按照实施例1-3和对比例1-3的方法制备凝胶,使用顶空固相微萃取-气相色谱-质谱联用(HS-SPME-GC-MS)的方法测试上述各组凝胶中香气物质的保留率(%),以实施例1为例,具体方法包括:
(1)取1g按照实施例1的方法制得的凝胶、1.8g NaCl、50U果胶裂解酶和5mL超纯水混合后密封于棕色顶空小瓶中混匀,恒温25℃放置20min,再以45℃、500rpm/min的搅拌下平衡15min,使用SPME萃取纤维(divinylbenzene/carboxen/polydimethylsiloxane)在40℃下吸附10min以提取挥发性香气成分。然后将纤维转移到GC进样口,在230℃的温度下解析5分钟。进样模式为不分流进样,使用HP-5色谱柱(30m×0.32mm×0.25μm)对挥发性香气成分进行分离。氦气流速设置为1.5mL/min。升温程序如下:40℃,保持2min,然后以4℃/min的速度升至120℃,再以7℃/min的速度升至200℃,之后以50℃/min的速度升至250℃,保持2min,最后冷却至初始温度。质谱的电子电离模式为70eV,扫描范围为35–400m/z,扫描速率为3.0scans/s。质谱的离子源温度和四极杆温度分别为230℃和250℃,测得凝胶中挥发性香气含量,作为试验组。
(2)根据实施例1制得的凝胶的质量(记为m1)以及各实施例和对比例在制备凝胶过程中所加入的香气物质的质量(记为m2),计算单位质量(1g)凝胶中香气物质的质量w=m2/m1×1g。然后采用wg香气物质(对于实施例1-2和对比例1-3来说均为柠檬烯,对于实施例3来说为月桂烯)替代步骤(1)的凝胶并按照步骤(1)相同的方法测试挥发性香气含量,作为对照组。
计算香气物质的保留率:保留率(%)=各试验组挥发性香气的含量/相对应的对照组的挥发性香气含量。
结果见表1所示。
表1香气物质的保留率(%)
由上表可知,相比于对比例1-3来说,本发明实施例1-3能够显著提升香气物质的保留率。
实验例2
分别取实施例1-3和对比例1-3制得的橙汁50mL,密封于聚乙烯瓶中在4℃下冷藏50天,分别于不同时间取样使用顶空固相微萃取-气相色谱-质谱联用(HS-SPME-GC-MS)的方法测试上述各组凝胶中香气物质的保留率(%),以实施例1为例,具体方法包括:
(1)取1g按照实施例1的方法制得的凝胶、1.8g NaCl和5mL超纯水混合后密封于棕色顶空小瓶中混匀,恒温25℃,20min,再以45℃、500rpm/min的搅拌下平衡15min,使用SPME萃取纤维(divinylbenzene/carboxen/polydimethylsiloxane)在40℃下吸附10min以提取挥发性香气成分。然后将纤维转移到GC进样口,在230℃的温度下解析5min。进样模式为不分流进样,使用HP-5色谱柱(30m×0.32mm×0.25μm)对挥发性香气成分进行分离。氦气流速设置为1.5mL/min。升温程序如下:40℃,保持2min,然后以4℃/min的速度升至120℃,再以7℃/min的速度升至200℃,之后以50℃/min的速度升至250℃,保持2min,最后冷却至初始温度。质谱的电子电离模式为70eV,扫描范围为35–400m/z,扫描速率为3.0scans/s。质谱的离子源温度和四极杆温度分别为230℃和250℃,测得凝胶中挥发性香气含量,作为试验组1。
(2)根据实施例1制得的凝胶的质量(记为m1)以及制备凝胶过程中所加入的香气物质的质量(记为m2),计算单位质量(1g)凝胶中香气物质的总质量w=m2/m1×1g。采用wg香气物质(对于实施例1-2和对比例1-3来说均为柠檬烯,对于实施例3来说为月桂烯)替代步骤(1)的凝胶按照步骤(1)相同的方法测试挥发性香气含量,作为对照组1。
计算香气物质的释放率,释放率(%)=各试验组挥发性香气的含量/相对应的对照组的挥发性香气含量。
结果见表2。
表2香气物质的释放率(%)
由上表可知,相比于对比例1-3来说,本发明实施例1-3制得的凝胶具有缓释效果,50天释放率达到50%以上。
显然,上述实施例仅仅是为清楚地说明所作的举例,而并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。
Claims (10)
1.一种包埋香气物质的缓释凝胶的制备方法,其特征在于,包括如下步骤,
S1步骤:将果胶与盐溶液混合,得到第一混合液;
S2步骤:将第一混合液与香气物质混合,调节pH值为1-3,在温度为60-100℃下静置,离心,获得凝胶。
2.根据权利要求1所述的包埋香气物质的缓释凝胶的制备方法,其特征在于,所述果胶的质量与盐溶液的体积比为0.1-7:100。
3.根据权利要求1或2所述的包埋香气物质的缓释凝胶的制备方法,其特征在于,所述香气物质选自柠檬烯、巴伦西亚橘烯、水芹烯、月桂烯、蒎烯、桧烯、罗勒烯、萜品油烯、松油烯、榄香烯、石竹烯、壬醛和乙酸乙酯中的至少一种;和/或,所述果胶与香气物质的质量比为104-108:1。
4.根据权利要求1-3中任一所述的包埋香气物质的缓释凝胶的制备方法,其特征在于,所述盐溶液选自氯化钠水溶液和/或柠檬酸钠水溶液;优选地,按照质量百分数计,所述盐溶液的浓度为0.05-20wt%。
5.根据权利要求1-4中任一所述的包埋香气物质的缓释凝胶的制备方法,其特征在于,S1步骤和/或S2步骤中,在200-3000rpm的搅拌下进行混合,混合时间为5-60min。
6.根据权利要求1-5中任一所述的包埋香气物质的缓释凝胶的制备方法,其特征在于,S2步骤中,静置时间至少为5min,优选为5-30min。
7.根据权利要求1-6中任一所述的包埋香气物质的缓释凝胶的制备方法,其特征在于,S2步骤中,混合之前还包括将第一混合液的pH值调为5-7,然后在温度为20-35℃的条件下与果胶甲酯酶反应的步骤;和/或,离心步骤之前还包括加入金属盐溶液混合后再静置的步骤;和/或,S2步骤之后还包括对凝胶进行干燥获得凝胶粉的步骤。
8.权利要求1-7中任一所述的包埋香气物质的缓释凝胶的制备方法制得的凝胶或者由所述的凝胶干燥后得到的凝胶粉。
9.权利要求1-7中任一所述的包埋香气物质的缓释凝胶制备方法制得的凝胶或者由所述的凝胶干燥后得到的凝胶粉在食品中的应用。
10.一种食品,其特征在于,包括权利要求8所述的凝胶或者凝胶粉,优选地,所述食品选自饮料或者果酱,饮料选自果蔬汁饮料、茶饮料或者乳饮料;优选地,所述食品中还包括果胶裂解酶。
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