CN113057340A - 一种菌菇膳食纤维改性方法 - Google Patents
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Abstract
本发明公开了一种菌菇膳食纤维改性方法,具体制备步骤包括:步骤1、菌菇膳食纤维预处理,步骤2,菌菇膳食纤维在碱性环境下与N,N‑二甲基酰胺反应;步骤3,加入环氧丙烷和乙醇混合液,搅拌,加入辛胺反应;步骤4,调节溶液酸碱度至中性;步骤5,先用去离子水洗三次,再用无水乙醇洗三次,烘干得到具有氨基基团的菌菇膳食纤维;步骤6,将具有氨基基团的菌菇膳食纤维在DMSO反应环境下加入1H‑吡唑‑1‑甲脒盐酸盐、N,N‑二异丙基乙胺充分反应;步骤7,先用去离子水洗三次,再用无水乙醇洗三次,烘干、研磨得胍基基团膳食纤维。本发明引入了胍基基团,得到的膳食纤维粒径更小,表面更加疏松多孔,其持水力、持油能力、对胆固醇吸附能力均有很大提高。
Description
技术领域
本发明涉及减肥降脂食品技术领域,具体的说是一种菌菇膳食纤维改性方法。
背景技术
香菇属于担子菌纲、口蘑科、香菇属,是世界上第二大食用菌,同样也是我国特产之一。我国每年香菇的产量大约300万吨,因其具有独特的口味经常成为人们餐桌上的美味佳肴。香菇中含有大量的营养成分,如蛋白质、维生素、矿物元素、膳食纤维。膳食纤维包括β-葡聚糖、几丁质、半纤维素等,其中β-葡聚糖是香菇膳食纤维中重要的组成部分。不溶性膳食纤维的含量非常的高,占干物质含量的70%左右,可溶性膳食纤维含量比较少,仅占干物质含量1.6%~2.8%左右。香菇柄虽然营养成分相对减少,不溶性膳食纤维的含量相对增多,是改性的良好材料。
专利号为CN104223123B的发明专利公开了一种富含益生菌的杏鲍菇膳食纤维的制备方法,具体包括加入酒精浸泡、加无机碱溶液水解和加入酸溶液酸水解,采取酸法和碱法结合的方式,得到水不溶性杏鲍菇膳食纤维,最终制得富含益生菌的杏鲍菇膳食纤维,然而并没有改善杏鲍菇膳食纤维的吸附能力。
发明内容
为了解决上述问题,本发明提供了一种能够提高膳食纤维吸附能力的膳食纤维制备方法。
为了达到上述目的,本发明是通过以下技术方案来实现的:
本发明是一种菌菇膳食纤维改性方法,具体制备步骤包括:步骤1、菌菇膳食纤维预处理:取干燥的香菇柄进行机械粉碎,过80~100目,得到菌菇粉,并进行干燥杀菌处理;
步骤2,取菌菇粉加入到反应装置内,每克菌菇粉加入5-8mlN,N-二甲基酰胺,在碱性环境下,40-80℃反应5-7h;
步骤3,步骤2反应结束后,再按照每克菌菇粉加入2-3ml环氧丙烷和1-1.500ml无水乙醇的比例加入环氧丙烷和无水乙醇的混合液,搅拌3-10min,按照每克菌菇粉加入3-4.5ml的辛胺的比例加入辛胺反应10-15h;
步骤4,向步骤3所得的溶液中加入浓度为3-5mol/l盐酸溶液调节溶液酸碱度,直至溶液呈中性;
步骤5,向步骤4所得的溶液中加入4倍体积去离子水充分混匀,离心,弃上清,再重复两次,再将4倍体积的去离子水换成4倍体积的无水乙醇重复三次,烘干得到具有氨基基团的菌菇膳食纤维;
步骤6,将具有氨基基团的菌菇膳食纤维在DMSO反应环境下按照每100mg氨基基团菌菇膳食纤维加入60-90mg1H-吡唑-1-甲脒盐酸盐和70-105μl 的N,N-二异丙基乙胺的比例加入1H-吡唑-1-甲脒盐酸盐和N,N-二异丙基乙胺充分反应20-30 h,其中,每100mg具有氨基基团的菌菇膳食纤维加入10-15ml的DMSO;
步骤7,向步骤6所得的溶液中加入4倍体积的去离子水充分混匀,离心,弃上清,再重复两次,再将去离子水换成无水乙醇重复三次,烘干,研磨至粉,得到具有胍基基团的膳食纤维。
本发明的进一步改进在于:步骤3中环氧丙烷与乙醇的体积比为2∶1。
本发明的进一步改进在于:步骤2中是通过加入浓度为40-60%的氢氧化钠溶液实现7<PH< 7.5。
本发明的进一步改进在于:步骤5和步骤7中烘干用的设备采用真空烘干箱,温度为60℃,烘干时间为24h。
本发明的进一步改进在于:步骤5和步骤7中离心处理的转速为8000rmp ,离心时间为15min。
本发明的进一步改进在于:步骤6中1H-吡唑-1-甲脒盐酸盐、具有氨基基团的菌菇膳食纤维的质量比为(0.5-0.8)∶1。
本发明的有益效果是:在反应过程中加入的N,N-二甲基酰胺、环氧丙烷、辛胺、1H-吡唑-1-甲脒盐酸盐、N,N-二异丙基乙胺均是过量的,反应结束后通过去离子水和无水乙醇洗掉多余反应物即可。本发明的膳食纤维引入胍基基团,改性后的膳食纤维粒径更小,表面更加疏松多孔,更有利于对油脂和胆固醇的吸附。经过对改性后的膳食纤维的理化特性检测,发现胍基基团膳食纤维的理化特性,即持水力、持油能力、对胆固醇吸附能力均有很大提高。
附图说明
图1是化学改性后菌菇膳食纤维的FTIR光谱图。
图2是未改性菌菇膳食纤维显微镜下放大图。
图3是氨基改性膳食纤维显微镜下放大图。
图4是胍基基团膳食纤维显微镜下放大图。
图5是化学改性后菌菇膳食纤维与对照组持水力的统计图。
图6是化学改性后菌菇膳食纤维与对照组的持油力统计图。
图7是化学改性后菌菇膳食纤维与对照组的吸附胆固醇能力统计图。
图8是动物实验大鼠体重变化图。
其中:图3-5中1表示未改性菌菇膳食纤维,2表示氨基改性膳食纤维,3表示胍基基团膳食纤维。
具体实施例
以下将以图式揭露本发明的实施方式,为明确说明起见,许多实务上的细节将在以下叙述中一并说明。然而,应了解到,这些实务上的细节不应用以限制本发明。也就是说,在本发明的部分实施方式中,这些实务上的细节是非必要的。
下面结合附图对本发明的技术方案做进一步的详细说明 :
实施例1
如图1-8所示,本发明是一种菌菇膳食纤维改性方法,具体制备步骤包括:步骤1、菌菇膳食纤维预处理:取干燥的香菇柄进行机械粉碎,过80~100目,得到菌菇粉,干燥杀菌处理;
步骤2,取2g菌菇粉加入到反应装置内,在PH值为7.1的弱碱性环境下与10mlN,N-二甲基酰胺40℃反应5h;
步骤3,步骤2反应结束后,再加入4ml环氧丙烷和2ml乙醇混合液,搅拌5min,加入6ml辛胺反应10h;
步骤4,向步骤3所得的溶液中加入3mol/l的盐酸溶液调节溶液酸碱度,直至溶液呈中性;
步骤5,向步骤4所得的溶液中加入4倍体积去离子水充分混匀,离心,弃上清,再重复两次,再将4倍体积去离子水换成4倍体积无水乙醇重复三次,烘干得到具有氨基基团的菌菇膳食纤维,其中,离心处理的转速为8000rmp ,离心时间为15min,烘干采用真空烘干箱,温度为60℃,烘干时间为24h;
步骤6,将300mg具有氨基基团的菌菇膳食纤维在30mlDMSO反应环境下加入180mg1H-吡唑-1-甲脒盐酸盐、210μlN,N-二异丙基乙胺充分反应20 h;
步骤7,向步骤6所得的溶液中加入4倍体积的去离子水充分混匀,离心,弃上清,再重复两次,再将去离子水换成无水乙醇重复三次,烘干,研磨至粉,得到具有胍基基团的膳食纤维,其中,离心处理的转速为8000rmp ,离心时间为15min,烘干采用真空烘干箱,温度为60℃,烘干时间为24h。
实施例2,
步骤2中取4g菌菇粉,加入质量分数50% NaOH溶液5.5ml,即5.5gNaOH颗粒加5.5ml去离子水,加入N,N-二甲基酰胺的体积为25ml,60℃反应6h;步骤3中加入的环氧丙烷的体积为10ml,无水乙醇为5ml,注射到反应体系中,搅拌5min,加入辛胺15ml反应12h;步骤6中,取400mg胍基基团膳食纤维,1H-吡唑-1-甲脒盐酸盐的加入量为293.16mg,N,N-二异丙基乙胺的体积为348.35μl,DMSO体积为50ml,充分反应24 h。其余步骤与实施例1相同。
实施例3
步骤2取25g菌菇粉,在pH为7.4的环境下,加入N,N-二甲基酰胺的体积为140ml,40℃反应5h,步骤3中加入的环氧丙烷的体积为75ml,无水乙醇为37.5ml,注入到反应体系中,搅拌10min,加入112.5ml辛胺,反应15h;步骤4加入5mol/l的盐酸溶液调节溶液酸碱度,直至溶液呈中性;步骤6,取1200mg具有氨基基团的菌菇膳食纤维,加入180mlDMSO、1080mg1H-吡唑-1-甲脒盐酸盐、1260μlN,N-二异丙基乙胺充分反应。其余具体操作与实施例2相同。
对胍基基团膳食纤维进行理化特性测试,即测试其持水力、持油能力、对胆固醇吸附能力;
1、测胍基基团膳食纤维的持水力(WHC):
取m1为1g膳食纤维,加入50ml去离子水,静置2h,将多余水滤除,称量剩余残渣质量m2,计算得出其持水力为
2、测胍基基团膳食纤维的持油力(OHC)
取m1为1g膳食纤维加入10g饱和脂肪酸(猪油)或不饱和脂肪酸(花生油)充分混匀,37℃静置2h,将溶液离心20min 转速4000rpm去掉上层油,称量剩余残渣质量m3,计算得出其持油力为
3、测胍基基团膳食纤维的胆固醇吸附能力:
所需试剂:
邻苯二甲醛试剂:20mg邻苯二甲醛加无水乙醇溶至20ml冷藏;
混合酸:冰乙酸和浓硫酸1:1混合;
标准胆固醇工作液(0.1mg/ml):胆固醇100mg溶于冰乙酸1L;
取m1为1g膳食纤维加入标准工作液10ml,37℃,6h,用酶标仪测550nm处测OD值。
动物实验:
造模期,模型组和药物组均喂高脂饲料30天构建高脂模型,建模成功后对模型组中的高脂大鼠进行治疗,采用灌胃,定期测体重,取血测血脂,对药物组中的高脂大鼠投喂胍基基团膳食纤维。整个实验过程大鼠均无异样,产品对大鼠无毒无害。实验结果如表1和表2所示:
表1:
表2:
其中,n =3,与模型组相比 *p<0.05,**p<0.01
表1中,对模型组、胍基DF组、阳性对照组的实验鼠投喂高脂饲料30天构建高脂模型,构建好模型后,胍基DF组的实验鼠投喂胍基基团膳食纤维,正常组的实验鼠一直正常喂养,模型组的实验鼠投喂正常食物,阳性对照组的实验鼠投喂掺有辛伐他汀的正常食物,辛伐他汀的量按 4mg/kg.bw提供;建模完成后,各组实验鼠体重如图8所示。由表1和2数据可得,药物组的实验鼠的血脂指标相对于模型组的实验鼠的血脂指标更好。
以上所述,仅为本发明中的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉该技术的人在本发明所揭露的技术范围内,可理解想到的变换或替换,都应涵盖在本发明的包含范围之内,因此,本发明的保护范围应该以权利要求书的保护范围为准。
Claims (5)
1.一种菌菇膳食纤维改性方法,其特征在于:具体制备步骤包括:步骤1、菌菇膳食纤维预处理:取干燥的香菇柄进行机械粉碎,过80~100目,得到菌菇粉,并进行干燥杀菌处理;
步骤2,取菌菇粉加入到反应装置内,每克菌菇粉加入5-8mlN,N-二甲基酰胺,在碱性环境下,40-80℃反应5-7h;
步骤3,步骤2反应结束后,再按照每克菌菇粉加入2-3ml环氧丙烷和1-1.500ml无水乙醇的比例加入环氧丙烷和无水乙醇的混合液,搅拌3-10min,按照每克菌菇粉加入3-4.5ml的辛胺的比例加入辛胺反应10-15h;
步骤4,向步骤3所得的溶液中加入浓度为3-5mol/l的盐酸溶液调节溶液酸碱度,直至溶液呈中性;
步骤5,向步骤4所得的溶液中加入4倍体积去离子水充分混匀,离心,弃上清,再重复两次,再将4倍体积的去离子水换成4倍体积的无水乙醇重复三次,烘干得到具有氨基基团的菌菇膳食纤维;
步骤6,将具有氨基基团的菌菇膳食纤维在DMSO反应环境下按照每100mg氨基基团菌菇膳食纤维加入60-90mg1H-吡唑-1-甲脒盐酸盐和70-105μl 的N,N-二异丙基乙胺的比例加入1H-吡唑-1-甲脒盐酸盐和N,N-二异丙基乙胺充分反应20-30 h,其中,每100mg具有氨基基团的菌菇膳食纤维加入10-15ml的DMSO;
步骤7,向步骤6所得的溶液中加入4倍体积的去离子水充分混匀,离心,弃上清,再重复两次,再将去离子水换成无水乙醇重复三次,烘干,研磨至粉,得到具有胍基基团的膳食纤维。
2.根据权利要求1所述一种菌菇膳食纤维改性方法,其特征在于:步骤2中是通过加入浓度为40-60%的氢氧化钠溶液实现7<PH<7.5。
3.根据权利要求2所述一种菌菇膳食纤维改性方法,其特征在于:步骤3中所述环氧丙烷与无水乙醇的体积比为2∶1。
4.根据权利要求3所述一种菌菇膳食纤维改性方法,其特征在于:步骤5和步骤7中烘干采用真空烘干箱,温度为60℃,烘干时间为24h。
5.根据权利要求4所述一种菌菇膳食纤维改性方法,其特征在于:步骤5和步骤7中离心处理的转速为8000rmp ,离心时间为15min。
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