CN1070693C - 防腐剂和防腐方法 - Google Patents

防腐剂和防腐方法 Download PDF

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CN1070693C
CN1070693C CN97190936A CN97190936A CN1070693C CN 1070693 C CN1070693 C CN 1070693C CN 97190936 A CN97190936 A CN 97190936A CN 97190936 A CN97190936 A CN 97190936A CN 1070693 C CN1070693 C CN 1070693C
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soluble hemicellulose
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CN1198078A (zh
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中村彰宏
服部光男
前田裕一
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Fuji Oil Co Ltd
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Abstract

食品与饮料的防腐剂，它含有水溶性的半纤维素作为活性成分；而另一类防腐剂，它则含有(A)水溶性的半纤维素和(B)，(B)为下列物质中的一种或几种，包括乙醇、甘氨酸、葡糖酸-δ-内酯、山梨酸、对-羟基苯甲酸、苯甲酸、脱氢乙酸、次氯酸及上述酸相应的盐，有机酸象醋酸、富马酸、己二酸、丙酸、山梨酸及上述酸相应的盐，低级脂肪酸酯、糖酯、多熔素、鱼精蛋白、溶菌酶、日本芥菜子的提取液、绿芥菜提取液、漂白面粉、脱乙酰壳多糖和肌醇六磷酸；防腐的方法，即应用上述防腐剂去保存食品和饮料类目标产品。

Description

防腐剂和防腐方法
技术领域
此发明是有关于防腐剂和防腐方法。
背景技术
有机酸、无机酸、乙醇和甘氨酸通常被用来防腐及延长食品的保存期(日本未经审查的专利，No.56-109580,57-43668,58-138367)。
近年来，各种食品都经筛选以寻找食品防腐剂，结果发现了许多防腐剂，如多熔素、鱼精蛋白、溶菌酶等以及合成的化学品。但是，由于这些防腐剂所表现出来的强抗菌活性仅仅是抑制某一种特定的细菌，因此，它们无法满足作为通用食品防腐剂的要求。为了得到满意的防腐效果，就必需向食品中加大量的这类防腐物质，而这是不理想的，因为其高昂的价格会提高总的成本。
除了这些物质外，有报道长期被用于食品的香料也含有具有抗菌活性的物质，但是它们同样不能完全满足作为食品防腐剂所需的条件。
如上所述，优选的用于食品和饮料的防腐剂应能在加入最小量的情况下就能长期起到保质抗菌效果，并且当在食品中使用时，一定不能破坏食品的味道和结构。
由于广泛用作食品防腐剂的象乙醇、甘氨酸、有机酸和无机酸，它们本身就带有特征性的味道和香气，因此它们不能以提供足够的防腐效果所需的量添加到食品和饮料中。同样，天然物质象多熔素、鱼精蛋白和溶菌酶的抗菌种类也非常少，因此当它们对某一特定细菌表现出强大抗菌活性的同时，对于引起食物腐败的大多数微生物却不起作用，所以它们也不能被用作满意的防腐剂。
发明的公开
在上述事实情况下，通过辛勤的研究，本发明者终于发现水溶性半纤维素，尤其是豆类中提取的水溶性半纤维素，表现出抗菌活性，可以有效地用作食品和饮料的防腐剂。特别指出的是，水溶性半纤维素对水分活性(AW)为0.8或更高的食品有效，例如象捏合的海产品(AW=0.8或更高)，生面条(AW=0.85)和蔬菜沙拉(AW=0.9或更高)。当水溶性半纤维素被用作食品和饮料的防腐剂时，只少量就可获得满意的抗菌活性，而且通过发明者进一步努力的研究，结果发现联合使用乙醇、甘氨酸、山梨酸、苯甲酸和它们的盐，有机酸象醋酸、富马酸、己二酸及它们的盐，低级脂肪酸酯、糖酯、多熔素、鱼精蛋白、溶菌酶、芥菜的提取液、辣根提取液、脱乙酰壳多糖等等的水溶性半纤维素可明显地提高抗菌活性。本发明就是基于这些发现而完成的。
换言之，本发明提供了以水溶性半纤维素为有效成分的防腐剂，及含有(A)水溶性半纤维素和(B)为有效成分的防腐剂，其中(B)为下列物质中的一种或几种，包括乙醇、甘氨酸、山梨酸、苯甲酸及上述酸相应的盐，有机酸象醋酸、富马酸、己二酸及上述酸相应的盐，低级脂肪酸酯、糖酯、多熔素、鱼精蛋白、溶菌酶、芥菜提取液、辣根提取液、脱乙酰壳多糖和肌醇六磷酸，以及防腐方法包括联合使用(A)水溶性半纤维素和(B),(B)为下列物质中的一种或几种，包括乙醇、甘氨酸、山梨酸、苯甲酸及上述酸相应的盐，有机酸象醋酸、富马酸、己二酸及上述酸相应的盐，低级脂肪酸酯、糖酯、多熔素、鱼精蛋白、溶菌酶、芥菜提取液、辣根提取液、脱乙酰壳多糖和肌醇六磷酸。应用本发明的最佳方式
按照本发明所述，水溶性半纤维素优选从豆类提取而来，更优选是大豆，尤其优选猪耳草。优选蛋白含量低的大豆半纤维素，尤其优选蛋白含量不超过5％。
水溶性半纤维素可以为任意分子量，但以高分子物质为优选，更优选的是平均分子量为几千到几百万的，而以分子量5000到一百万为尤其优选。如果分子量太大，会使粘度增加，而使工艺操作性能降低。水溶性半纤维素的平均分子量的值由限制粘度的方法决定，在该方法中以标准短根霉多糖(Showa Denko,KK.的产品)作为标准物质来测定0.1M NaNO3的粘度。糖醛酸的测定用Blumenkrantz方法进行，中性糖的测定是经醛醇乙酰化后用GLC方法进行。
水溶性半纤维素可以从含有半纤维素的原料经水提法得到，必要的话也可以在酸或碱的条件下进行热洗脱得到，或者也可以通过酶降解的方法洗脱得到。下面的就是一个生产水溶性半纤维素方法的例子。
合适的原料来源于植物，包括去除了油和蛋白的大豆、棕榈、椰子、谷类或棉籽的油性种子的壳，以及谷类象大米或小麦经去除淀粉和其它部分后剩下的渣滓。如果原料是大豆，那么豆腐渣(制备豆腐的副产品)和豆浆或分离大豆蛋白也可以被利用。
这些原料可热降解，优选温度为80℃-130℃，更优选温度为100℃-130℃，在酸或碱性条件下，但以接近每一种蛋白的等电点的pH为优选，水溶部分经分馏后，可直接干燥或者是经活性炭处理，树脂吸收处理或乙醇沉淀去除了疏水物质或低分子物质后，再干燥成水溶性的半纤维素。也可以用半纤维酶或果胶酶进行降解提取。
水溶性半纤维素是一种多糖，其糖组分包括半乳糖、阿拉伯糖、木糖、岩藻糖、葡萄糖、鼠李糖和半乳糖醛酸。通过水解得到的水溶性半纤维素的组分的详细分析可在日本未经审查的公开中请No.4-325058中找到。
分子量大的水溶性半纤维素其分子量与粘度成一定比例，因此粘度可作为一个指标来限定用作食品和饮料防腐剂的水溶性半纤维素的适用的分子量范围。也就是说，按照本发明，用作防腐剂的水溶性半纤维素在25℃10％水溶液中优选粘度为10mPa·s或更高(在25℃10％水溶液中用Brookfield旋转粘度仪测量)，更优选粘度为50mPa·s或更高，最优选粘度为80mPa·s或更高。只要水溶性半纤维素的溶液粘度低于1000mPa·s就可以使用。
本发明中的水溶性半纤维素可单独用作防腐剂，或者可与一种或几种已知化合物联合使用以提高抗菌活性。适用的物质范围将在下面讨论。
乙醇和甘氨酸可以是适合于添加到食品中的各种等级。山梨酸和苯甲酸的盐类具有钠盐或者是钾盐，以钾盐为优选。有机酸象醋酸、富马酸和己二酸或它们的盐也可以是适合于添加到食品中的各种等级品。所用的低级脂肪酸酯可以是己酸、辛酸、癸酸或月桂酸的甘油酯。所用糖酯可以是各种适用的食品添加剂。所用鱼精蛋白可以是鱼精蛋白的硫酸盐或盐酸盐。所用的芥菜提取液或辣根提取液可以是芥子油的脂溶组分。脱乙酰壳多糖为适用于一般食品的商业品，可以游离形式或以醋酸盐、谷氨酸盐的形式使用。肌醇六磷酸应是一种适用于一般食品的商业品。
添加到食品或其它产品中的水溶性半纤维素的量取决于其组分的组合，而没有特别的限制，其使用的优选范围为约0.05-15％(以重量计)。
发明中的防腐剂的添加方法没有限制，补充物质可根据需要决定是否添加。如果需要添加，可与水溶性半纤维素一起加到食品或饮料中去，或者也可分别加入。如果发明中的水溶性半纤维素以水溶性的形式使用，它可以喷到食品或饮料产品表面，或者将产品浸到水溶液中。
在添加防腐剂的时间上没有特别的限制，水溶性半纤维素可以所期望的任何方法加到食品或饮料中去。因此，它可以在食品或饮料的生产过程中的任何一步添加，例如如果在生产过程中添加，可在热定型后、包装前，将食品或饮料产品浸泡到水溶液中或将水溶液喷到产品上面。
对于防腐剂所适用的食品没有特别的限制，例如可提到的谷类、水果、蔬菜、海藻和以上述食物为主要成分的家庭盘菜、泡菜，也适用于捏合的海产品象煮熟的鱼糊、chikuwa鱼糊、捣碎的鱼糕、鱼肉火腿和香肠以及肉类产品象熏肉、汉堡包和肉球，豆浆和豆腐，听装果汁和咖啡；以水分活性(AW)为0.8或更高的食品和饮料为特别适合。
尽管发明人对发明中的防腐剂的抗菌活性的表达机理并不完全清楚，但是其抗菌活性的提高在后面的例子中却得到充分的证明。
现在本发明将通过实例给出更为详细的解释。实例中所用的水溶性半纤维素按下列方法制备。水溶性大豆半纤维素的制备
向分离大豆蛋白过程中得到的豆腐渣粗品中加入2倍量的水，用盐酸调pH到4.5后，将混合物在120℃加热1小时，提取水溶性大豆半纤维素。提取后，将混合物离心(5000G离心10分钟)，主要含有水溶性大豆半纤维素的水溶部分被分离开。向以这种方式获得的含有水溶性大豆半纤维素的水溶液中加入氢氧化钠，调pH至12。然后将混合物在70加热30分钟。弃去加热产生的沉淀，溶液用盐酸中和(pH7)。得到的水溶性大豆半纤维素溶液用透析法脱盐，通过一根活性炭柱处理后，将其干燥制成水溶性大豆半纤维素。
水溶性半纤维素终产物中组分的比率和糖的组成如下所示：
水溶性大豆半纤维素的组分比率(重量百分比)
水                          5.4
蛋白粗品                    9.1
灰分粗品含量                6.3
多糖类                     79.0
平均分子量                 207,000
粘度1)                    56.8
 1)粘度：cPs,10％水溶液
水溶性大豆半纤维素的糖的组成(重量百分比)
半乳糖醛酸           17.6
鼠李糖                2.6
岩藻糖                1.9
阿拉伯糖             20.5
半乳糖               49.9
木糖                  6.4
葡萄糖                1.1例1
对通过水溶性半纤维素与可增加其抗菌活性的物质的联合使用而使抗菌活性增加进行了研究。抗菌活性用一种标准培养基(pH7.2)来检测，培养基中带有水溶性半纤维素，其量在0％、0.5％、1.0％或足够量，并含有可增加其抗菌活性的物质，以大肠杆菌、米曲霉、植物乳杆菌或酿酒酵母为菌株。抗菌活性的判别是通过用细菌来感染培养基，37℃下培养4天，并测定浊度来进行的。当细菌增殖时，培养基的浊度会增加，因此如果检测物质具有抗菌活性，细菌的增殖就会受到抑制，从而限制了浊度的增加。浊度通过测定610nm波长处的可见光的吸收值来测量(使用PTL-396S分光光度计，Nihon Spectroscopy的产品)，浊度单位按照JIS1010的方法来确定。专门指出的是，将含有1ppm高岭土的水的浊度定为1个单位。结果如下。水溶性半纤维素被证明具有强的防腐能力。抗大肠杆菌(Escherichia coli)活性
实验组             保存天数
    1     2     3     4
没有附加物水溶性半纤维素同上 0.5％1.0％  1521914  5265645 268119 468258
只加入乙醇同上乙醇+水溶性半纤维素(0.5％) 0.05％0.1％0.05％1.0％  125111429  458415248107 492453358 472
只加入甘氨酸同上甘氨酸+水溶性半纤维素(0.5％) 0.5％1.0％0.5％1.0％  12796115  4193984722 48722997 401215
只加入抗坏血酸钠盐同上抗坏血酸钠盐+水溶性半纤维素(0.5％) 0.1％0.5％0.1％0.5％  10812140  3812562180 41843618 75
只加入甘油脂肪酸酯同上甘油脂肪酸酯+水溶性半纤维素(0.5％) 0.01％0.05％0.01％0.05％  1245450  3952504914 48129352 412239
只加入常用盐同上常用盐+水溶性半纤维素(0.5％) 1.0％2.0％1.0％2.0％  13210188  5003754834 329325 500500
只加入辣根提取液同上辣根提取液+水溶性半纤维素(0.5％) 0.1％0.5％0.1％0.5％  157120  7918280  17612511421  33821615926
抗米曲霉(Aspergillus oryzae)活性
实验组            保存天数
    1     2     3     4
没有附加物水溶性半纤维素同上 0.5％1.0％  289117104  587356245 479
只加入乙醇同上乙醇+水溶性半纤维素(0.5％) 0.05％0.1％0.05％1.0％  2315129  158115144107  398292393358 439472
只加入甘氨酸同上甘氨酸+水溶性半纤维素(0.5％) 0.5％1.0％0.5％1.0％  107768145  219178127132  428382299193 491375
只加入抗坏血酸钠盐同上抗坏血酸钠盐+水溶性半纤维素(0.5％) 0.1％0.5％0.1％0.5％  121724436  38919625987 478498298 465
只加入甘油脂肪酸酯同上甘油脂肪酸酯+水溶性半纤维素(0.5％) 0.01％0.05％0.01％0.05％  119798642  495275247184 475453352
只加入常用盐同上常用盐+水溶性半纤维素(0.5％) 1.0％2.0％1.0％2.0％  82625432  418245198114 485351305 500500
只加入辣根提取液同上辣根提取液+水溶性半纤维素(0.5％) 0.1％0.5％0.1％0.5％  329280  89276829  22419510789  379289298127
抗植物乳杆菌(Lactobacillus Plantarm)活性
实验组               保存天数
    1     2     3     4
没有附加物水溶性半纤维素同上 0.5％1.0％  1204124     22615995     418379178 487352
只加入乙醇同上乙醇+水溶性半纤维素(0.5％) 0.05％0.1％0.05％1.0％  41114011     254185215126     482372311343 461
只加入甘氨酸同上甘氨酸+水溶性半纤维素(0.5％) 0.5％1.0％0.5％1.0％  113712546     32919710588 314236141 417274
只加入抗坏血酸钠盐同上抗坏血酸钠盐+水溶性半纤维素(0.5％) 0.1％0.5％0.1％0.5％  108574412     21112911923     36231221378 325113
只加入甘油脂肪酸酯同上甘油脂肪酸酯+水溶性半纤维素(0.5％) 0.01％0.05％0.01％0.05％  734950     2912375329 39114168 315227
只加入常用盐同上常用盐+水溶性半纤维素(0.5％) 1.0％2.0％1.0％2.0％  97241811     3983446834 12297 370289
只加入辣根提取液同上辣根提取液+水溶性半纤维素(0.5％) 0.1％0.5％0.1％0.5％  10790     4117180     14310311124  31720520136
抗酿酒酵母(Saccharomyces cerevisiae)活性
实验组              保存天数
    1     2     3     4
没有附加物水溶性半纤维素同上 0.5％1.0％  2592917  5126629 10796 212147
只加入乙醇同上乙醇+水溶性半纤维素(0.5％) 0.05％0.1％0.05％1.0％  15193230  4582054213 4189527 141119
只加入甘氨酸同上甘氨酸+水溶性半纤维素(0.5％) 0.5％1.0％0.5％1.0％  8958104  2131684613  3883019754 458196107
只加入抗坏血酸钠盐同上抗坏血酸钠盐+水溶性半纤维素(0.5％) 0.1％0.5％0.1％0.5％  11748120  3861961170 40129620 95
只加入甘油脂肪酸酯同上甘油脂肪酸酯+水溶性半纤维素(0.5％) 0.01％0.05％0.01％0.05％  1024950  3771291911 39111648 208171
只加入常用盐同上常用盐+水溶性半纤维素(0.5％) 1.0％2.0％1.0％2.0％  10418177  3963594628 11966 192105
只加入辣根提取液同上辣根提取液+水溶性半纤维素(0.5％) 0.1％0.5％0.1％0.5％  10500  581390  112751811  1541115827
如以上结果所示，水溶性半纤维素不仅与无添加物组相比表现出天然的良好的防腐效能，而且与到目前为止已知具有抗菌活性的物质相比也同样表现出天然的良好的防腐效能，而这些抗菌物质与水溶性半纤维素结合使用则具有了更强的防腐性能。例2
下面列出的每一种防腐剂都被加到一种基本混合物中，这种混合物是通过将50g常用盐、150g淀粉、15g谷氨酸钠、20g糖和1.5kg冰水加到3kg冷冻的碾碎的熏鲱鱼肉中制备而来的(关于这种基本混合物，加入的每一种组分各自的比例按照重量百分比在下面也有列出)。将每一种混合物100g装到1,1-二氯乙烯膜中去并且在90℃的热水中加热30分钟后，将其放入流水中冷却40分钟，制成熟的鱼糊卷。每个实验组合有10个鱼糊卷，将其放在30℃的培养箱中保存，通过目测观察质量保持的程度来决定防腐的性能。结果如下。
防腐剂1 A  B  C  D  E  F  G  H
没有添加物
 1(对照组) 0.5
 2(对照组) 0.5
 3(对照组) 0.5
 4(对照组) 0.05
 5(对照组) 0.05
 6(对照组) 0.05
 7(对照组) 0.5
 8(实验组) 0.5
 9(实验组) 0.5  0.5
 10(实验组) 0.5  0.5
 11(实验组) 0.5  0.5
 12(实验组) 0.5  0.05
 13(实验组) 0.5  0.05
 14(实验组) 0.5  0.05
 15(实验组) 0.5  0.5
注1：
A：水溶性半纤维素
B：乙醇
C：甘氨酸
D：抗坏血酸钠盐
E：甘油脂肪酸酯
F：多熔素
G：溶菌酶
H：辣根提取液防腐结果
防腐剂1                                 保存天数
    1     2     3     4     5     6     7     8
没有添加物 2/10 10/10
 1(对照组) 1/10  4/10  10/10
 2(对照组) 0/10  3/10  8/10  10/10
 3(对照组) 1/10  4/10  7/10 10/10
 4(对照组) 0/10  3/10  8/10 10/10
 5(对照组) 0/10  3/10  6/10  8/10 10/10
 6(对照组) 0/10  4/10  7/10  9/10 10/10
 7(对照组) 0/10  0/10  1/10  2/10  5/10  6/10 10/10
 8(实验组) 0/10  0/10  0/10  2/10  5/10  7/10  10/10
 9(实验组) 0/10  0/10  1/10  3/10  6/10  9/10 10/10
 10(实验组) 0/10  0/10  0/10  2/10  4/10  7/10 10/10
 11(实验组) 0/10  0/10  0/10  1/10  3/10  9/10 10/10
 12(实验组) 0/10  0/10  0/10  2/10  5/10  8/10  9/10 10/10
 13(实验组) 0/10  0/10  0/10  1/10  3/10  7/10 10/10
 14(实验组) 0/10  0/10  0/10  3/10  5/10  8/10 10/10
 15(实验组) 0/10  0/10  0/10  0/10  2/10  4/10  7/10 10/10
上面的结果清楚地显示，含有本发明中提到的防腐剂的实验组表现出高的保质性能。另外，没有观察到加入本发明的防腐剂对质量有相反的效果。例3
将500g小麦粉、10g常用盐和200mL水的混合物用碾子碾成一个长的面团，并用传统方法制成生面条。按下面所述方法进一步处理后，将样品放在无菌的陪替氏培养皿中，盖好，然后在35℃，相对湿度85％的条件下进行防腐实验。(A)对照组(没有附加物)(B)在和面过程中加入1.0％水溶性半纤维素(C)在和面过程中加入0.5％水溶性半纤维素，成形，煮熟，在1.0％的水溶性半纤维素的水溶液中浸泡10秒钟，去水。(D)制备煮熟的面条，然后在1.0％的水溶性半纤维素的水溶液中浸泡10秒钟，去水。
防腐实验结果如下：
    实验组                              贮存时间
    10     20     30     42     66     80     100
A(对照组)    -    -    +   ++
B(实验组)    -    -    -   -   + ++
C(实验组)    -    -    -   -   - + ++
D(实验组)    -    -    -   +   ++
符号-：没有变化
+：出现微生物，局部软化
++：出现微生物，局部溶解
这些结果明显地证明了实验组(B)、(C)和(D)的优越性。例4
按下面所列的组分制备土豆沙拉。实验样品制备中加入0.5％水溶性半纤维素，加或不加0.3％醋酸钠，2个对照组，一个没有附加物，一个只加了0.3％醋酸钠。实验样品放在20℃保存，并对每一种的保质性进行比较，结果如下所示。
土豆沙拉的组成(按重量比)
土豆泥           55
蛋黄酱           15
胡罗卜           15
黄瓜             10
盐               1
胡椒             0.5所用方法：(A)无附加物(B)加入0.5％醋酸钠(C)加入0.5％水溶性半纤维素(D)加入0.5％水溶性半纤维素和0.3％醋酸钠防腐结果
实验组               贮存时间
    1     2     3     4     5
 A(对照组)   -   +   ++
B(对照组)   -   -   + ++
C(实验组)   -   -   - + ++
D(实验组)   -   -  - + ++
符号-：没有变化
+：出现微生物，局部软化
++：出现微生物，局部溶解
这些结果明显地证明了本发明中实验组的优越性。
工业应用性
从上面可以看出，本发明所述的防腐剂在用于食品和饮料时，甚至加入少量就可表现出足够的防腐效能，以熟鱼糊为例，与不加本发明的防腐剂的情况相比，鱼糊的保存期延长了5倍，并且没有破坏其味道、组织或产生不期望的气味。另外，对于熟面条的保存，将其浸泡在1.0％含有发明中的防腐剂的水溶液中，可以抑制微生物的增殖，在制备生面条的过程中加入1.0％的防腐剂也可起到防腐的效果。因此，既然在食品和饮料的制备过程中，向其原料中加入防腐剂就可获得足够的防腐效能，防腐剂在其处理方面也具有优越性。此外，本发明中的防腐剂可与其它物质结合使用，象乙醇、甘氨酸、赖氨酸和甘油脂肪酸酯，以提高防腐效能，也可作为天然防腐剂用在除食品外的化妆品和药品中。

Claims (2)

1．一种含有提取自大豆的水溶性半纤维素作为有效成分的食品与饮料的防腐剂。
2．一种防腐方法，它包括将0.05至15％重量的提取自大豆的水溶性半纤维素添加至食品或饮料中。
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CN107439901A (zh) * 2017-09-06 2017-12-08 太仓市荣德生物技术研究所 一种生物环保型杀菌剂
CN107373286A (zh) * 2017-09-11 2017-11-24 太仓市荣德生物技术研究所 一种使用量小效果好的生物防腐剂
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