CN112690329A - 一种多维改性氧化淀粉基涂膜果蔬保鲜剂及制备方法 - Google Patents
一种多维改性氧化淀粉基涂膜果蔬保鲜剂及制备方法 Download PDFInfo
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- CN112690329A CN112690329A CN202010742078.6A CN202010742078A CN112690329A CN 112690329 A CN112690329 A CN 112690329A CN 202010742078 A CN202010742078 A CN 202010742078A CN 112690329 A CN112690329 A CN 112690329A
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- ultrasonic
- potato
- starch
- extraction
- potato peel
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Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/16—Coating with a protective layer; Compositions or apparatus therefor
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/14—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10
- A23B7/153—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of liquids or solids
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/14—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10
- A23B7/153—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of liquids or solids
- A23B7/154—Organic compounds; Microorganisms; Enzymes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G5/00—Alkaloids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/04—Extraction or purification
- C08B30/048—Extraction or purification from potatoes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/18—Oxidised starch
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/64—Fats; Fatty oils; Ester-type waxes; Higher fatty acids, i.e. having at least seven carbon atoms in an unbroken chain bound to a carboxyl group; Oxidised oils or fats
- C12P7/6436—Fatty acid esters
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Abstract
本发明公开了一种多维改性氧化淀粉基涂膜果蔬保鲜剂及制备方法,该保鲜剂包括如下重量百分比的原料:马铃薯氧化淀粉:2.0~3.0%、马铃薯皮醇提物:1.0~2.0%、马铃薯皮生物碱:0.4~0.6%、玉米秸秆芯低聚木糖:0.2~0.4%、猪油单甘脂:1.0~2.0%、棕榈酸:1.0~1.5%、甘油:1.0~2.0%、纯水88.5~93.4%。本发明以超声、微波及次氯酸三维一体的改性方式得到的氧化马铃薯淀粉为基质,通过添加纯天然抑菌物质以及猪油单甘脂、棕榈酸及甘油辅助材料,经缓慢交合、剪切均质、冷却、包装得成品。本发明制备的果蔬保鲜剂既安全环保、又有利于人类健康,是一种无毒、抑菌、抗氧化、成膜性好的天然果蔬保鲜剂,同时本发明为解决副产物的综合开发利用提供了新途径。
Description
技术领域
本发明涉及果蔬保鲜技术领域,具体涉及一种多维改性氧化淀粉基涂膜果蔬保鲜剂及制备方法。
背景技术
新鲜果蔬采收后仍然进行着呼吸和蒸腾作用,容易产生皱缩、萎焉,同时易被微生物侵染而出现腐烂变质的现象。目前部分涂膜果蔬保鲜剂不仅含有对人体有害的化学成分,而且成膜性、保水性差。本方法利用纯绿色天然食物为原料,通过不同物质间的相互作用,研发安全环保的新型果蔬保鲜剂,既有利于保障人类健康,又能为副产物的综合开发利用提供新径。
淀粉是生物合成的最丰富的可再生资源,是一种价格低廉、可生物降解的天然高分子聚合物,淀粉膜具有柔韧性好、透明度高、透气率低等优点,但其机械强度差,通过化学改性,可以改变淀粉的结构及其性质,增强其成膜性。氧化淀粉是一种变性淀粉,其在氧化剂作用下将分子中的羟基转化成羧基和羰基,进而使其具有透明度高、粘度低、糊化温度低、老化程度低、成膜性和流动性好的特点。我国是世界上马铃薯种植面积最大,产量最高的国家,改性的马铃薯淀粉,被广泛应用于食品行业。
黄酮类化合物是一种重要的生理活性物质,具有抑菌、抗癌、抗氧化等生物活性。黄酮类化合物的抑菌活性主要与黄酮芳环上的羟基数量与位置有关。绿原酸是由咖啡酸与奎尼酸组成的缩酚酸,是多酚的主要成分,具有抗氧化、抗菌、抗病毒、升高白细胞、免疫调节、抗肿瘤、降血压、降血脂等作用。糖苷生物碱是茄科植物中进行新陈代谢过程所产生的二级产物,具有抗菌、抗病毒、降低胆固醇等生物活性。我国马铃薯产量居世界首位,70~80%用于鲜食或进行深加工,产生近百万吨的马铃薯皮渣。近年来虽有部分研究者将马铃薯皮渣用来制沼气或饲料,但多数作为废弃物丢掉,不但浪费资源,而且对环境造成了污染。有研究报道,马铃薯皮中含有黄酮、绿原酸及糖苷生物碱等成分,特别是通过不同极性乙醇介质提取的醇提物,使它们具有很强的抑菌活性。为其发展成为高效、无毒的天然果蔬保鲜剂提供了现实依据。植物源保鲜剂是天然提取物,它具有无残留、无公害、无污染、不易产生抗药性等优点,被公认为是世界上的绿色保鲜剂,可广泛应用于直接食用的果蔬保鲜。
低聚木糖是由2-7个木糖分子以α-1,4糖苷键结合而成,耐热、耐酸性强,甜度比蔗糖和葡萄糖低,能够促进钙吸收、抗龋齿、抑菌以及改善肠道益生菌等功能。玉米芯中含有35%的半纤维素,其组成主要为木聚糖,可以通过降解生产低聚木糖。因此,以价廉易得的玉米秸秆芯为原料,将其开发出的低聚糖应用于果蔬保鲜方面具有很大市场开发前景。
复合型变性淀粉基涂膜果蔬保鲜剂是多种原料综合利用的新型研究成果,可有效提高和拓展副产物的综合利用,提高各类抑菌物质的协同作用,在纯天然果蔬保鲜剂开发方面具有广阔的发展前景。
发明内容
本发明的目的是为了得到一种抑菌性、阻湿性、增塑性较强的涂膜果蔬保鲜剂。
本发明利用氧化马铃薯淀粉经适度糊化后加入几种纯天然抑菌剂以及阻湿剂、增塑剂,经保温孵化,搅拌均匀冷却后制备涂膜果蔬保鲜剂的方法,是通过以下步骤实现的:
一、一种多维改性氧化淀粉基涂膜果蔬保鲜剂包括下述重量百分比的原料:
马铃薯氧化淀粉:2.0~3.0%;
马铃薯皮醇提物:1.0~2.0%;
马铃薯皮生物碱:0.4~0.6%;
玉米秸秆芯低聚木糖:0.2~0.4%;
猪油单甘脂:1.0~2.0%;
棕榈酸:1~1.5%;
甘油:1.0~2.0%;
余量为纯水。
二、其制备方法如下:
1.制备马铃薯氧化淀粉:选取黑龙江地区粘度偏低、淀粉产量较高的品种克新13号,需贮藏期在120天以上,经破碎、过滤、沉淀、反复洗涤,取沉淀物离心,于40℃真空减压干燥制备,要求淀粉含量为82%以上。将一定质量的马铃薯淀粉与水混溶,调成40%的淀粉乳,置于超声、微波环境中,设置超声功率150~200W,超声10~15min后改为微波环境,微波输出功率700~800W,3~5min后随即再改为超声环境,依次循环,总计100min。期间以不间断逐滴加入的形式添加次氯酸钠,次氯酸钠的总用量为淀粉重量的1.2~1.4%,用0.5mol/L的盐酸保持反应溶液pH9.0~9.5,反应结束后用0.5mol/L的盐酸调pH至6.5~7.0。氧化后的马铃薯淀粉匀浆低温离心,离心力为6000~8000g,温度为0~4℃,时间为10~15min。沉淀物经纯净水反复清洗离心置表面皿,再由真空干燥箱于85℃、真空度≥0.09MPa真空干燥2~3h得马铃薯氧化淀粉成品;
2.制备马铃薯皮醇提物:取贮藏期在120天以上的马铃薯,表皮清洗后采用专用削皮器轻取马铃薯表面皮层,皮层厚度要求为0.15~0.5mm。马铃薯皮经以液氮作为研磨介质的冷冻粉碎机粉碎过80目筛,按照浸提媒介极性减弱的原则采用三段式逐步提取。第一阶段超高压乙醇浸提,将冷冻粉碎的马铃薯皮粉用45~50%乙醇以料液比1∶6装入双层聚乙烯塑料袋中,并抽去多余空气,置于300~400MPa、50℃高静压条件下浸提50~60min。第二阶段采用双极超声复提,将上述浸提样品倒入烧杯内,并添加适量95%的乙醇,使得浸提液的最终乙醇浓度为65~70%,然后固定于超声浸提设备中,同时再将超声细胞破碎仪超声探头插入烧杯内的液面以下,构成内外双极超声模式。其外极超声浸提槽超声频率40KHz,输出功率180~200W,温度45~50℃,烧杯内超声探头设置频率20KHz,输出功率400~500W,同时开启内外超声设备复提30~40min。第三阶段超临界二氧化碳补提,将上述浸提样品经3500~4000g离心15~20min后,浸提液备用,固体残渣装入超临界二氧化碳反应釜中,设置反应温度45~50℃,反应釜压力200~300bar,夹带剂采用75~80%乙醇,静态提取30~40min后,设置二氧化碳流量2.5L/h进行动态超临界萃取,直至样品收集口无液态样品流出为止。合并上述浸提液,通过真空旋转蒸发仪浓缩,并经氮吹至膏状后置超低温冰箱冷冻,由真空冷冻干燥机冷冻干燥12~16h得马铃薯皮醇提物;
3.制备马铃薯皮生物碱:取贮藏期在120天以上的马铃薯,表皮清洗后采用专用削皮器轻取马铃薯表面皮层,皮层厚度要求为0.15~0.5mm,低温烘干后粉碎过60目筛。取马铃薯皮粉按1∶30(g∶mL)料液比加入0.5%~1.0%的硫酸溶液,置于微波-紫外-超声三位一体浸提设备中,微波输出功率360W,输出形式每间隔60s微波加热3~5min,同时超声工作频率28KHz,输出功率580W提取10~15min后,超声工作频率变为27KHz,输出功率380W再提取10~15min后,工作频率变为26KHz,输出功率180W再提取10~15min,完成变频提取。滤液加28%氨水调pH至析出沉淀后于离心力4000~4500g离心10~15min,沉淀以2~3倍体积的甲醇溶解,于离心力4000~4500g离心15~20min,上清液减压浓缩至膏状,经氮吹仪,控制分压表于0.3~0.4MPa,氮吹直至膏状变干,吹走残留甲醇。将半干的马铃薯生物碱置真空干燥箱于50℃、真空度≥0.09MPa真空干燥8~12h得马铃薯皮生物碱成品;
4.制备玉米秸秆芯低聚木糖:将已去叶、毛根的玉米秸秆切成50mm长的无节小段,并从中间劈开,得到玉米秸秆芯,粉碎过60目筛。取玉米秸秆芯粉以1∶25(g∶mL)的料液比加入0.3~0.5mol/L的NaOH溶液,超声频率20KHz,输出功率380W,温度50~60℃,超声碱提30~40min后于离心力3500~4000g条件下离心20~30min,取上清液用0.5mol/L盐酸调pH为5.0~5.5,加1~2倍体积无水乙醇4℃醇沉后于离心力3000~3500g条件下离心20~30min,沉淀经氮气吹干得木聚糖粗品。将木聚糖粗品加入到pH4.0~5.0的柠檬酸缓冲液中,使料液比达到1∶20(g∶mL),料液加热至50℃后,添加底物1~2%的木聚糖酶(42000U/g),迅速置于微波反应器中,每隔30s微波1min,设定微波功率480W,脉动微波酶解30~45min,结束后以沸水浴灭酶8~10min,再于3500~4000g离心20~30min,将得到的低聚木糖溶液置于旋转蒸发仪上,减压浓缩至膏状,转至真空干燥箱内,于55℃真空干燥得低聚木糖干粉,再经超音速气流粉碎设备进行超微细化,使其粒度范围D50为0.5~10μm;
5.制备猪油单甘脂:取猪背脂肪精炼的猪油,与甘油以摩尔比1∶1混合,加入12~14%固定化脂肪酶Lipozyme RM IM(275U/g),混合均匀后与一定量撕成棉絮状的脱脂棉混合,使其充分的尽可能多且均匀地附着于脱脂棉絮之上,附着程度以拿起不自然滴油为准,并将其轻轻置于超临界反应釜中,填充量不超过反应釜体积的四分之三,进行超临界CO2条件下保压联合酶解,反应压力200bar,反应温度45~50℃、保压反应20~24h,打开排气阀,设置二氧化碳流量0.5L/h进行动态超临界萃取,直至无液体流出为止,制得猪油酶解物;
将猪油酶解物加入分子蒸馏设备中,设置进料速度2kg/h,蒸发温度175℃,蒸馏压力40Pa,刮膜机转速350rpm,一级分子蒸馏后将重相进行二级分子蒸馏,设置进料速度2kg/h,蒸发温度210℃,蒸馏压力25Pa,刮膜机转速350rpm。再次将轻相按照一、二级分子蒸馏程序循环往复一次,即得猪油单甘脂样品;
6.按照配方比例,合并马铃薯皮醇提物、马铃薯皮生物碱以及玉米芯低聚木糖,且以纯净水配置成天然抑菌溶液后,加入马铃薯氧化淀粉制备天然抑菌淀粉乳溶液,于水浴温度0~4℃,振荡器转速100r/min条件下陈化2~3h;
7.按照配方比例,将猪油单甘脂、棕榈酸及甘油三种辅料混合后以内剪切高速均浆机6000~8000r/min均浆1~2min制备复合辅料;
8.将天然抑菌淀粉乳溶液在75~85℃水浴中加热,不断搅拌进行糊化,30~40min后缓慢加入上述已制备好的复合辅料,并加速搅拌3~5min,保温孵化10~15min后,转入剪切高速匀浆机中,在1000~1200r/min条件下低速均浆15~20min,装入包装袋中采用真空包装技术获得成品。
本发明的一种多维改性氧化淀粉基涂膜果蔬保鲜剂,以超声、微波及次氯酸三维一体的改性方式得到的透明度高、成膜性好、老化程度低的氧化马铃薯淀粉为基质,通过添加马铃薯皮醇提物、马铃薯皮生物碱以及玉米芯低聚木糖三种纯天然物质,提高保鲜剂的抑菌性能,再通过添加猪油单甘脂增强膜的阻湿和保湿性能,同时添加的甘油增加了膜的韧性。采用本发明制备的果蔬保鲜剂既安全环保、又有利于人类健康,是一种具备无毒、抑菌、抗氧化成膜性好的天然果蔬保鲜产品,同时为解决副产物的综合开发利用提供了新途径。
具体实施方式
实施例1按照下列步骤制备本发明的涂膜果蔬保鲜剂:
1.制备马铃薯氧化淀粉:选取黑龙江地区粘度偏低、淀粉产量较高的品种克新13号,需贮藏期在120天以上,经破碎、过滤、沉淀、反复洗涤,取沉淀物离心,于40℃真空减压干燥制备,要求淀粉含量为82%以上。将200g的马铃薯淀粉与300mL水混溶,调成淀粉乳,置于超声、微波环境中,设置超声功率150W,超声15min后改为微波环境,微波输出功率700W,5min后随即再改为超声环境,依次循环,总计100min。期间以不间断逐滴加入的形式添加次氯酸钠,次氯酸钠的总用量为2.4g,用0.5mol/L的盐酸保持反应溶液pH9.0,反应结束后用0.5mol/L的盐酸调pH至6.5。氧化后的马铃薯淀粉匀浆低温离心,离心力为6000g,温度为0~4℃,时间15min。沉淀物经纯净水反复清洗离心置表面皿,再由真空干燥箱于85℃、真空度≥0.09MPa真空干燥3h得马铃薯氧化淀粉成品;
2.制备马铃薯皮醇提物:取贮藏期在120天以上的马铃薯,表皮清洗后采用专用削皮器轻取马铃薯表面皮层,皮层厚度要求为0.15~0.5mm。马铃薯皮经以液氮作为研磨介质的冷冻粉碎机粉碎过80目筛,按照浸提媒介极性减弱的原则采用三段式逐步提取。第一阶段超高压乙醇浸提,取100g马铃薯皮粉与600mL 45%的乙醇混合后装入双层聚乙烯塑料袋中,抽去多余空气,置于300MPa、50℃高静压条件下浸提60min。第二阶段采用双极超声复提,将上述浸提样品倒入烧杯内,加入400mL 95%的乙醇,使得浸提液的最终乙醇浓度为65%,然后固定于超声浸提设备中,同时将超声细胞破碎仪超声探头插入烧杯内的液面以下,构成内外双极超声模式。其外极超声浸提槽超声频率40KHz,输出功率180W,温度50℃,烧杯内超声探头设置频率20KHz,输出功率400W,同时开启内外超声设备复提30min。第三阶段超临界二氧化碳补提,将上述浸提样品经3500g离心20min后,浸提液备用,固体残渣装入超临界二氧化碳反应釜中,设置反应温度50℃,反应釜压力200bar,夹带剂采用75%乙醇,静态提取30min后,设置二氧化碳流量2.5L/h进行动态超临界萃取,直至样品收集口无液态样品流出为止。合并上述浸提液,通过真空旋转蒸发仪浓缩,并经氮吹至膏状后置超低温冰箱冷冻,由真空冷冻干燥机冷冻干燥12h得马铃薯皮醇提物;
3.制备马铃薯皮生物碱:取贮藏期在120天以上的马铃薯,表皮清洗后采用专用削皮器轻取马铃薯表面皮层,皮层厚度要求为0.15~0.5mm,低温烘干后粉碎过60目筛。取100g马铃薯皮粉加入0.5%的硫酸溶液3000mL,置于微波-紫外-超声三位一体浸提设备中,微波输出功率360W,输出形式每间隔60s微波加热3min,同时超声工作频率28KHz,输出功率580W提取15min后,超声工作频率变为27KHz,输出功率380W再提取10min后,工作频率变为26KHz,输出功率180W再提取10min,完成变频提取。滤液加28%氨水调pH至析出沉淀后于离心力4000g离心15min,沉淀以3倍体积的甲醇溶解,于离心力4000g离心20min,上清液减压浓缩至膏状,经氮吹仪,控制分压表于0.3~0.4MPa,氮吹直至膏状变干,吹走残留甲醇。将半干的马铃薯生物碱置真空干燥箱于50℃、真空度≥0.09MPa真空干燥12h得马铃薯皮生物碱成品;
4.制备玉米秸秆芯低聚木糖:将已去叶、毛根的玉米秸秆切成50mm长的无节小段,并从中间劈开,得到玉米秸秆芯,粉碎过60目筛。取玉米秸秆芯粉200g,加入0.3mol/L的NaOH溶液5000mL,置于超声波发生器中,超声频率20KHz,输出功率380W,温度50℃,超声碱提40min后于离心力3500g条件下离心20min,取上清液用0.5mol/L盐酸调pH为5.0,加1倍体积无水乙醇4℃醇沉后于离心力3000g条件下离心30min,沉淀经氮气吹干得木聚糖粗品。将木聚糖粗品10g加入到200mL pH4.0的柠檬酸缓冲液中,料液加热至50℃后,添加底物1.0%的木聚糖酶(42000U/g),迅速置于微波反应器中,每隔30s微波1min,设定微波功率480W,脉动微波酶解30min后以沸水浴灭酶8min,再于3500g离心20min,将得到的低聚木糖溶液置于旋转蒸发仪上,减压浓缩至膏状,转至真空干燥箱内,于55℃真空干燥得低聚木糖干粉,再经超音速气流粉碎设备进行超微细化,使其粒度范围D50为0.5~10μm;
5.制备猪油单甘脂:取猪背脂肪精炼的猪油100g,与10g甘油混合,加入12g固定化脂肪酶Lipozyme RM IM(275U/g),混合均匀后与一定量撕成棉絮状的脱脂棉混合,使其充分的尽可能多且均匀地附着于脱脂棉絮之上,附着程度以拿起不自然滴油为准,并将其轻轻置于超临界反应釜中,填充量不超过反应釜体积的四分之三,进行超临界CO2条件下保压联合酶解,反应压力200bar,反应温度45℃、保压反应20h,打开排气阀,设置二氧化碳流量0.5L/h进行动态超临界萃取,直至无液体流出为止,制得猪油酶解物;
将猪油酶解物加入分子蒸馏设备中,设置进料速度2kg/h,蒸发温度175℃,蒸馏压力40Pa,刮膜机转速350rpm,一级分子蒸馏后将重相进行二级分子蒸馏,设置进料速度2kg/h,蒸发温度210℃,蒸馏压力25Pa,刮膜机转速350rpm。再次将轻相按照一、二级分子蒸馏程序循环往复一次,即得猪油单甘脂样品;
6.将所得马铃薯皮醇提物1.0g、马铃薯皮生物碱0.4g以及玉米芯低聚木糖0.2g加入到93.4g纯净水中,配置成天然抑菌溶液后,加入2.0g马铃薯氧化淀粉于水浴温度0~4℃,振荡器转速100r/min条件下陈化2h,制备成天然抑菌淀粉乳溶液;
7.将所得猪油单甘脂1.0g、棕榈酸1.0g及甘油1.0g三种辅料混合后以内剪切高速均浆机6000r/min均浆1min制备复合辅料;
8.将得到的天然抑菌淀粉乳溶液在75℃水浴中加热,不断搅拌进行糊化,30min后缓慢加入上述已制备好的复合辅料,并加速搅拌3min,保温孵化10min后,转入剪切高速均浆机中,在1000r/min条件下低速均浆15min,装入包装袋中采用真空包装技术获得成品。
实施例2按照下列步骤制备本发明的涂膜果蔬保鲜剂:
1.制备马铃薯氧化淀粉:选取黑龙江地区粘度偏低、淀粉产量较高的品种克新13号,需贮藏期在120天以上,经破碎、过滤、沉淀、反复洗涤,取沉淀物离心,于40℃真空减压干燥制备,要求淀粉含量为82%以上。将200g的马铃薯淀粉与300mL水混溶,调成淀粉乳,置于超声、微波环境中,设置超声功率200W,超声10min后改为微波环境,微波输出功率800W,3min后随即再改为超声环境,依次循环,总计100min。期间以不间断逐滴加入的形式添加次氯酸钠,次氯酸钠的总用量为2.8g,用0.5mol/L的盐酸保持反应溶液pH9.5,反应结束后用0.5mol/L的盐酸调pH至6.5。氧化后的马铃薯淀粉匀浆低温离心,离心力为8000g,温度为0~4℃,时间为10min。沉淀物经纯净水反复清洗离心置表面皿,再由真空干燥箱于85℃、真空度≥0.09MPa真空干燥3h得马铃薯氧化淀粉成品;
2.制备马铃薯皮醇提物:取贮藏期在120天以上的马铃薯,表皮清洗后采用专用削皮器轻取马铃薯表面皮层,皮层厚度要求为0.15~0.5mm。马铃薯皮经以液氮作为研磨介质的冷冻粉碎机粉碎过80目筛,按照浸提媒介极性减弱的原则采用三段式逐步提取。第一阶段超高压乙醇浸提,取100g马铃薯皮粉与600mL 50%的乙醇混合后装入双层聚乙烯塑料袋中,抽去多余空气,置于400MPa、50℃高静压条件下浸提50min。第二阶段采用双极超声复提,将上述浸提样品倒入烧杯内,加入480mL 95%的乙醇,使得浸提液的最终乙醇浓度为70%,然后固定于超声浸提设备中,同时将超声细胞破碎仪超声探头插入烧杯内的液面以下,构成内外双极超声模式。其外极超声浸提槽超声频率40KHz,输出功率200W,温度45℃,烧杯内超声探头设置频率20KHz,输出功率500W,同时开启内外超声设备复提40min。第三阶段超临界二氧化碳补提,将上述浸提样品经4000g离心15min后,浸提液备用,固体残渣装入超临界二氧化碳反应釜中,设置反应温度45℃,反应釜压力300bar,夹带剂采用80%乙醇,静态提取40min后,设置二氧化碳流量2.5L/h进行动态超临界萃取,直至样品收集口无液态样品流出为止。合并上述浸提液,通过真空旋转蒸发仪浓缩,并经氮吹至膏状后置超低温冰箱冷冻,由真空冷冻干燥机冷冻干燥16h得马铃薯皮醇提物;
3.制备马铃薯皮生物碱:取贮藏期在120天以上的马铃薯,表皮清洗后采用专用削皮器轻取马铃薯表面皮层,皮层厚度要求为0.15~0.5mm,低温烘干后粉碎过60目筛。取100g马铃薯皮粉加入1.0%的硫酸溶液3000mL,置于微波-紫外-超声三位一体浸提设备中,微波输出功率360W,输出形式每间隔60s微波加热5min,同时超声工作频率28KHz,输出功率580W提取10min后,超声工作频率变为27KHz,输出功率380W再提取15min后,工作频率变为26KHz,输出功率180W再提取15min,完成变频提取。滤液加28%氨水调pH至析出沉淀后于离心力4500g离心15min,沉淀以2倍体积的甲醇溶解,于离心力4500g离心15min,上清液减压浓缩至膏状,经氮吹仪,控制分压表于0.3~0.4MPa,氮吹直至膏状变干,吹走残留甲醇。将半干的马铃薯生物碱置于真空干燥箱于50℃、真空度≥0.09MPa真空干燥12h得马铃薯皮生物碱成品;
4.制备玉米秸秆芯低聚木糖:将已去叶、毛根的玉米秸秆切成50mm长的无节小段,并从中间劈开,得到玉米秸秆芯,粉碎过60目筛。取玉米秸秆芯粉200g,加入0.5mol/L的NaOH溶液5000mL,置于超声波发生器中,超声频率20KHz,输出功率380W,温度60℃,超声碱提30min后于离心力4000g条件下离心20min,取上清液用0.5mol/L盐酸调pH为5.0,加1倍体积无水乙醇4℃醇沉后于离心力3000g条件下离心20min,沉淀经氮气吹干得木聚糖粗品。将木聚糖粗品10g加入到200mL pH5.0的柠檬酸缓冲液中,料液加热至50℃后,添加底物2.0%的木聚糖酶(42000U/g),迅速置于微波反应器中,每隔30s微波1min,设定微波功率480W,脉动微波酶解45min后以沸水浴灭酶10min,再于4000g离心30min,将得到的低聚木糖溶液置于旋转蒸发仪上,减压浓缩至膏状,转至真空干燥箱内,于55℃真空干燥得低聚木糖干粉,再经超音速气流粉碎设备进行超微细化,使其粒度范围D50为0.5~10μm;
5.制备猪油单甘脂:取猪背脂肪精炼的猪油100g,与10g甘油混合,加入14g固定化脂肪酶Lipozyme RM IM(275U/g),混合均匀后与一定量撕成棉絮状的脱脂棉混合,使其充分的尽可能多且均匀地附着于脱脂棉絮之上,附着程度以拿起不自然滴油为准,并将其轻轻置于超临界反应釜中,填充量不超过反应釜体积的四分之三,进行超临界CO2条件下保压联合酶解,反应压力200bar,反应温度50℃、保压反应24h,打开排气阀,设置二氧化碳流量0.5L/h进行动态超临界萃取,直至无液体流出为止,制得猪油酶解物;
将猪油酶解物加入分子蒸馏设备中,设置进料速度2kg/h,蒸发温度175℃,蒸馏压力40Pa,刮膜机转速350rpm,一级分子蒸馏后将重相进行二级分子蒸馏,设置进料速度2kg/h,蒸发温度210℃,蒸馏压力25Pa,刮膜机转速350rpm。再次将轻相按照一、二级分子蒸馏程序循环往复一次,即得猪油单甘脂样品;
6.将所得马铃薯皮醇提物2.0g、马铃薯皮生物碱0.6g以及玉米芯低聚木糖0.4g加入到88.5g纯净水中,配置成天然抑菌溶液后,加入3.0g马铃薯氧化淀粉于水浴温度0~4℃,振荡器转速100r/min条件下陈化3h,制备成天然抑菌淀粉乳溶液;
7.将所得猪油单甘脂2.0g、棕榈酸1.5g及甘油2.0g三种辅料混合后以内剪切高速均浆机8000r/min均浆2min制备复合辅料;
8.将得到的天然抑菌淀粉乳溶液在85℃水浴中加热,不断搅拌进行糊化,40min后缓慢加入上述已制备好的复合辅料,并加速搅拌5min,保温孵化15min后,转入剪切高速均浆机中,在1200r/min条件下低速均浆20min,装入包装袋中采用真空包装技术获得成品。
Claims (2)
1.一种多维改性氧化淀粉基涂膜果蔬保鲜剂及制备方法,其特征在于:包括下述重量百分比的原料:
马铃薯氧化淀粉:2.0~3.0%;
马铃薯皮醇提物:1.0~2.0%;
马铃薯皮生物碱:0.4~0.6%;
玉米秸秆芯低聚木糖:0.2~0.4%;
猪油单甘脂:1.0~2.0%;
棕榈酸:1.0~1.5%;
甘油:1.0~2.0%;
余量为纯水。
2.如权利要求1所述的一种多维改性氧化淀粉基涂膜果蔬保鲜剂及制备方法,其特征在于:包括如下步骤:
一、制备马铃薯氧化淀粉
选取黑龙江地区粘度偏低、淀粉产量较高的品种克新13号,需贮藏期在120天以上,经破碎、过滤、沉淀、反复洗涤,取沉淀物离心,于40℃真空减压干燥制备,要求淀粉含量为82%以上。将一定质量的马铃薯淀粉与水混溶,调成40%的淀粉乳,置于超声、微波环境中,设置超声强度150~200W,超声10~15min后改为微波环境,微波输出功率700~800W,3~5min后随即再改为超声环境,依次循环,总计100min。期间以不间断逐滴加入的形式添加次氯酸钠,次氯酸钠的总用量为淀粉重量的1.2~1.4%,用0.5mol/L的盐酸保持反应溶液pH9.0~9.5,反应结束后用0.5mol/L的盐酸调pH至6.5~7.0。氧化后的马铃薯淀粉匀浆低温离心,离心力为6000~8000g,温度为0~4℃,时间为10~15min。沉淀物经纯净水反复清洗离心置表面皿,再由真空干燥箱于85℃、真空度≥0.09MPa真空干燥2~3h得马铃薯氧化淀粉成品;
二、制备马铃薯皮醇提物
取贮藏期在120天以上的马铃薯,表皮清洗后采用专用削皮器轻取马铃薯表面皮层,皮层厚度要求为0.15~0.5mm。马铃薯皮经以液氮作为研磨介质的冷冻粉碎机粉碎过80目筛,按照浸提媒介极性减弱的原则采用三段式逐步提取。第一阶段超高压乙醇浸提,将冷冻粉碎的马铃薯皮粉用45~50%乙醇以料液比1∶6装入双层聚乙烯塑料袋中,并抽去多余空气,置于300~400MPa、50℃高静压条件下浸提50~60min。第二阶段采用双极超声复提,将上述浸提样品倒入烧杯内,并添加适量95%的乙醇,使得浸提液的最终乙醇浓度为65~70%,然后固定于超声浸提设备中,同时再将超声细胞破碎仪超声探头插入烧杯内的液面以下,构成内外双极超声模式。其外极超声浸提槽超声频率40KHz,输出功率180~200W,温度45~50℃,烧杯内超声探头设置频率20KHz,输出功率400~500W,同时开启内外超声设备复提30~40min。第三阶段超临界二氧化碳补提,将上述浸提样品经3500~4000g离心15~20min后,浸提液备用,固体残渣装入超临界二氧化碳反应釜中,设置反应温度45~50℃,反应釜压力200~300bar,夹带剂采用75~80%乙醇,静态提取30~40min后,设置二氧化碳流量2.5L/h进行动态超临界萃取,直至样品收集口无液态样品流出为止。合并上述浸提液,通过真空旋转蒸发仪浓缩,并经氮吹至膏状后置超低温冰箱冷冻,由真空冷冻干燥机冷冻干燥12~16h得马铃薯皮醇提物;
三、制备马铃薯皮生物碱
取贮藏期在120天以上的马铃薯,表皮清洗后采用专用削皮器轻取马铃薯表面皮层,皮层厚度要求为0.15~0.5mm,低温烘干后粉碎过60目筛。取马铃薯皮粉按1∶30(g∶mL)料液比加入0.5%~1.0%的硫酸溶液,置于微波-紫外-超声三位一体浸提设备中,微波输出功率360W,输出形式每间隔60s微波加热3~5min,同时超声工作频率28KHz,输出功率580W提取10~15min后,超声工作频率变为27KHz,输出功率380W再提取10~15min后,工作频率变为26KHz,输出功率180W再提取10~15min,完成变频提取。滤液加28%氨水调pH至析出沉淀后于离心力4000~4500g离心10~15min,沉淀以2~3倍体积的甲醇溶解,于离心力4000~4500g离心15~20min,上清液减压浓缩至膏状,经氮吹仪,控制分压表于0.3~0.4MPa,氮吹直至膏状变干,吹走残留甲醇。将半干的马铃薯生物碱置真空干燥箱于50℃、真空度≥0.09MPa真空干燥8~12h得马铃薯皮生物碱成品;
四、制备玉米秸秆芯低聚木糖
将已去叶、毛根的玉米秸秆切成50mm长的无节小段,并从中间劈开,得到玉米秸秆芯,粉碎过60目筛。取玉米秸秆芯粉以1∶25(g∶mL)的料液比加入0.3~0.5mol/L的NaOH溶液,超声频率20KHz,输出功率380W,温度50~60℃,超声碱提30~40min后于离心力3500~4000g条件下离心20~30min,取上清液用0.5mol/L盐酸调pH为5.0~5.5,加1~2倍体积无水乙醇4℃醇沉后于离心力3000~3500g条件下离心20~30min,沉淀经氮气吹干得木聚糖粗品;将木聚糖粗品加入到pH4.0~5.0的柠檬酸缓冲液中,使料液比达到1∶20(g∶mL),料液加热至温度50℃后,添加底物1~2%的木聚糖酶(42000U/g),迅速置于微波反应器中,每隔30s微波1min,设定微波功率480W,脉动微波酶解30~45min,结束后以沸水浴灭酶8~10min,再于3500~4000g离心20~30min,将得到的低聚木糖溶液置于旋转蒸发仪上,减压浓缩至膏状,转至真空干燥箱内,于55℃真空干燥得低聚木糖干粉,再经超音速气流粉碎设备进行超微细化,使其粒度范围D50为0.5~10μm;
五、制备猪油单甘脂
取猪背脂肪精炼的猪油,与甘油以摩尔比1∶1混合,加入12~14%固定化脂肪酶Lipozyme RM IM(275U/g),混合均匀后与一定量撕成棉絮状的脱脂棉混合,使其充分的尽可能多且均匀地附着于脱脂棉絮之上,附着程度以拿起不自然滴油为准,并将其轻轻置于超临界反应釜中,填充量不超过反应釜体积的四分之三,进行超临界CO2条件下保压联合酶解,反应压力200bar,反应温度45~50℃、保压反应20~24h,打开排气阀,设置二氧化碳流量0.5L/h进行动态超临界萃取,直至无液体流出为止,制得猪油酶解物;
将猪油酶解物加入分子蒸馏设备中,设置进料速度2kg/h,蒸发温度175℃,蒸馏压力40Pa,刮膜机转速350rpm,一级分子蒸馏后将重相进行二级分子蒸馏,设置进料速度2kg/h,蒸发温度210℃,蒸馏压力25Pa,刮膜机转速350rpm。再次将轻相按照一、二级分子蒸馏程序循环往复一次,即得猪油单甘脂样品;
六、按照配方比例,合并马铃薯皮醇提物、马铃薯皮生物碱以及玉米芯低聚木糖,且以纯净水配置成天然抑菌溶液后,加入马铃薯氧化淀粉制备天然抑菌淀粉乳溶液,于水浴温度0~4℃,振荡器转速100r/min条件下陈化2~3h;
七、按照配方比例,将猪油单甘脂、棕榈酸及甘油三种辅料混合后以内剪切高速均浆机6000~8000r/min均浆1~2min制备复合辅料;
八、将天然抑菌淀粉乳溶液在75~85℃水浴中加热,不断搅拌进行糊化,30~40min后缓慢加入上述已制备好的复合辅料,并加速搅拌3~5min,保温孵化10~15min后,转入剪切高速均浆机中,在1000~1200r/min条件下低速均浆15~20min,装入包装袋中采用真空包装技术获得成品。
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