CN106977622A - 一种用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法 - Google Patents
一种用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法 Download PDFInfo
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Abstract
本发明公开了一种用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法。主要以壳聚糖和原儿茶酸分子作为反应底物，采用EDC介导的交联反应合成壳聚糖-原儿茶酸接枝共聚物。本发明的合成过程简单，所得的壳聚糖-原儿茶酸接枝共聚物的水溶性好，接枝率和抗氧化活性均较高，能显著提高食用菌的贮藏品质并延长货架期。本项发明可以解决壳聚糖水溶性差、抗氧化活性低等问题，从而改善壳聚糖的性能并扩大其在食品贮藏保鲜中的应用范围。该方法投入少，适合于大规模生产使用，具有极好的应用前景。
Description
技术领域
本发明属于食品科学领域，特别涉及一种用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法。
背景技术
壳聚糖又称脱乙酰甲壳素，是由自然界广泛存在的几丁质经过脱乙酰作用所得。壳聚糖无毒无污染易降解，并具有良好的吸附性、成膜性以及生物相容性，在食品、生物、农业等领域都有应用。壳聚糖作为一种天然多糖，其来源丰富，无毒、无污染，可在食品表面形成半透膜，能有效地抑制病菌入侵和生长，越来越受到人们的关注。但是，天然壳聚糖的水溶性较差且抗氧化活性较低，极大地限制了其应用范围。因此，需要对壳聚糖进行改性，合成具有强抗氧化活性的壳聚糖衍生物。由于壳聚糖分子上存在大量活泼的氨基和羟基，为其化学改性提供了可能。目前为止研究较多的壳聚糖衍生物有醚化、含氧无机酸酯化、季铵盐、N-酰化、金属配合物等，这些衍生物与壳聚糖相比，溶解性和抗氧化性能都得到了一定程度的改善。然而，上述壳聚糖衍生物的抗氧化活性并不高，若将该类衍生物作为抗氧化剂用于食品工程领域，难以产生良好的经济效益。
相比于传统化学改性方法，采用EDC介导的壳聚糖改性方法是将原儿茶酸接枝到壳聚糖分子的支链中，所得的壳聚糖-原儿茶酸接枝共聚物具有较高的抗氧化活性。现有的壳聚糖-酚酸接枝共聚物的合成方法主要采用1-乙基-3-(3-二甲基胺丙基)碳化二亚胺盐酸盐(EDAC)为交联剂，但该方法所得的产物接枝率低，不利于大规模生产应用。
发明内容
本发明的目的是提供一种用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法，将具有强抗氧化活性的酚酸改性壳聚糖的制备方法，并将合成的壳聚糖衍生物用于食用菌涂膜保鲜，以解决现有的壳聚糖衍生物抗氧化活性较低，不利于大规模生产应用的问题。
为实现上述目的，本发明采用如下技术方案：
一种用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法，其特征在于：以壳聚糖和原儿茶酸分子作为反应底物，在冰水浴环境中，采用EDC介导法合成壳聚糖-原儿茶酸接枝共聚物，并将接枝共聚物用于食用菌的涂膜保鲜。
具体步骤如下：
(1)将壳聚糖溶于乙酸溶液，磁力搅拌直至完全溶解，同时将原儿茶酸溶于乙醇；
(2)将EDC加入到含有MES缓冲液的反应器中；
(3)将步骤(1)所得的原儿茶酸溶液加入反应器中，立即加入N-羟基琥珀酰亚胺(NHS)并调节溶液pH值，随后置于冰水浴中反应，磁力搅拌；
(4)将步骤(1)所得的壳聚糖溶液加入反应器中，反应；
(5)将步骤(4)所得的反应液装入透析袋中，先用自来水透析，再用去离子水透析；
(6)将步骤(5)所得的透析液冷冻干燥后即得壳聚糖-原儿茶酸接枝共聚物；
(7)将步骤(6)所得的接枝共聚物配成水溶液，涂抹于食用菌表面。
优选的，步骤(3)中，溶液pH值为5.5，反应时间为1h。
优选的，步骤(4)中，在20℃下反应12h。
优选的，所述壳聚糖的浓度为5g/L，原儿茶酸的浓度为11.6g/L，EDC的浓度为43g/L，NHS的浓度为8.6g/L。
优选的，步骤(7)中，接枝共聚物涂膜液的浓度为10g/L。
优选的，本发明所述食用菌选用杏鲍菇。
本发明的有益效果是：本发明合成所得的壳聚糖-原儿茶酸接枝共聚物的接枝率和体外抗氧化活性均较高。本项发明可以解决壳聚糖在化学修饰过程中接枝率低、产品有污染等问题，可显著改善壳聚糖的水溶性和抗氧化活性，并扩大其应用范围。该方法投入少，适合于大规模生产使用，具有极好的应用前景。制备的壳聚糖-原儿茶酸接枝共聚物的接枝率为279.6mg/g，该接枝共聚物对DPPH自由基具有较高的清除活性，清除作用呈现剂量依赖关系，当接枝共聚物的浓度为5mg/mL时，最高清除率为92.52％。
附图说明
图1是壳聚糖-原儿茶酸接枝共聚物的核磁共振氢谱图。
图2是壳聚糖-原儿茶酸接枝共聚物对DPPH自由基的清除活性。
图3是壳聚糖-原儿茶酸接枝共聚物溶液对杏鲍菇贮藏过程中丙二醛含量的影响。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
壳聚糖-原儿茶酸接枝共聚物的合成过程：
(1)称取0.5g壳聚糖溶于25mL乙酸溶液，磁力搅拌直至完全溶解，同时称取1.16g原儿茶酸溶于3mL无水乙醇中；
(2)称取4.3g EDC溶于20mLMES缓冲液中，震荡使EDC完全溶解，；
(3)将完全溶解的原儿茶酸溶液加入反应器中，立即加入0.86g NHS并调节溶液pH值至5.5，随后置于冰水浴中，磁力搅拌反应1h；
(4)将完全溶解的壳聚糖溶液加入反应器中，20℃下反应12h；
(5)将反应液装入透析袋中，先用自来水透析48h，再用去离子水透析24h；
(6)将透析液冷冻干燥后即得壳聚糖-原儿茶酸接枝共聚物，为紫红色样品，其接枝率为279.6mg/g；
实施例2
壳聚糖-原儿茶酸接枝共聚物的结构和体外抗氧化活性测定：
(1)分别精确称取5mg的壳聚糖与壳聚糖-原儿茶酸接枝共聚物样品，溶于0.5mL重水中，25℃下测定其核磁共振氢谱。
(2)壳聚糖和壳聚糖-原儿茶酸接枝共聚物的1H NMR谱如图1所示，壳聚糖在δ＝1.7ppm处的峰对应于乙酰氨基葡萄糖残基的甲基质子，在δ＝3.3ppm处的峰对应于吡喃糖环C-3上的质子；在δ＝3.4ppm处的峰对应于吡喃糖环C-4上的质子；在δ＝3.7ppm处的峰对应于吡喃糖环C-5上的质子；在δ＝4.3ppm处的峰对应于吡喃糖环C-6上的质子；在δ＝2.8ppm处的微弱峰对应于C-2上的质子；在δ＝4.7ppm处的峰对应于C-1上的质子。而在壳聚糖-原儿茶酸接枝共聚物中，两个新的峰分别出现在δ＝6.68ppm和δ＝7.22ppm处，对应于原儿茶酸残基上的质子。这个结果进一步确认壳聚糖与原儿茶酸的成功接枝。
(3)测定壳聚糖-原儿茶酸接枝共聚物对DPPH自由基的清除活性，具体方法如下：称取接枝共聚物干燥粉末溶于蒸馏水中，配制成不同浓度的样品溶液(1-5mg/mL)，取2mL DPPH·乙醇溶液与2mL样品溶液混匀后，室温下放置30min，用无水乙醇调零，在517nm下测吸光值，记作A1。取2mL DPPH·乙醇溶液与2mL无水乙醇混匀后，室温下放置30min，用无水乙醇调零，在517nm下测吸光值，记作A0。取2mL无水乙醇溶液与2mL样品溶液混匀后，室温下放置30min，用无水乙醇调零，在517nm下测吸光值，记作A2。按照下式计算不同浓度受试物对DPPH自由基的清除率。
清除率(％)＝[A0–(A1–A2)]/A0×100
(4)壳聚糖-原儿茶酸接枝共聚物的DPPH自由基清除活性的结果如图2所示。壳聚糖-原儿茶酸接枝共聚物的DPPH自由基清除活性随着样品浓度的增加而增大，当样品浓度为5mg/ml时，接枝物的DPPH自由基清除活性达92.52％，而相同浓度壳聚糖的DPPH自由基清除活性仅为10.06％，结果表明，通过EDC介导的接枝共聚物反应合成壳聚糖-原儿茶酸接枝共聚物可显著增强天然壳聚糖的体外抗氧化活性。
实施例3
壳聚糖-原儿茶酸接枝共聚物对食用菌(杏鲍菇)的涂膜保鲜效果。
(1)食用菌采收当天置于5—8℃冷链运输装置中，并根部带培养基，运到实验室后立即处理。弃去根部培养基，选取菇体完整、颇色洁白、无病虫害、无机械伤、子实体大小基本一致的食用菌。
(2)将挑选45个食用菌随机分成3部分，即3种处理：分别用10g/L的壳聚糖-原儿茶酸接枝共聚物涂膜处理；用10g/L的壳聚糖涂膜处理；以及不作处理的空白组。使用大小为27cm×28cm的聚乙烯薄膜袋封口袋贮藏在湿度95％、4℃条件下贮藏，每个处理分5个小组(袋)，每3天取样一次，每次随机取样3个食用菌，切块后用液氮处理，-80℃下保存。
(3)取1.0g食用菌冷冻组织测定丙二醛含量。用5mL 5％(m/v)的三氯乙酸溶液冰浴研磨，然后离心20min(10000×g，4℃)。取1mL上清液与1mL 10％三氯乙酸溶液(含0.67％硫代巴比妥酸)混合，并将混合物在沸水浴加热20min(从溶液出现气泡开始计时)，冰浴冷却，离心10min(10000×g，4℃)。取上清液分别测定450cm、532nm、600nm处的吸光值，并按下式计算MDA含量：
MDA含量(umol/g)＝{[6.45(OD532－OD600)－0.56OD450]×V×(A/a)}/m
式中：A为反应液总量(mL)；V为提取液总量(mL)；a为测定提取液量(mL)；m为食用菌样品质量(g)。
(4)丙二醛是膜脂质过氧化作用的最终产物，也是评价食用菌膜脂质过氧化程度的重要指标之一。如图3所示，随着贮藏时间的延长，食用菌的MDA含量呈逐渐增加的趋势，贮藏至15d时，空白对照组食用菌的MDA含量达1.21umol/g，显著高于壳聚糖处理组(1.04umol/g)和接枝共聚物处理组(0.76umol/g)。在整个贮藏过程中，接枝共聚物处理组食用菌的MDA含量始终低于壳聚糖处理组和空白对照组，说明壳聚糖-原儿茶酸接枝共聚物可显著降低食用菌的脂质过氧化程度，从而延缓食用菌的衰老。
Claims (7)
1.一种用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法，其特征在于：以壳聚糖和原儿茶酸分子作为反应底物，在冰水浴环境中，采用1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐介导的交联反应合成具有强抗氧化活性的壳聚糖-原儿茶酸接枝共聚物，并将接枝共聚物用于食用菌的涂膜保鲜。
2.如权利要求1所述的用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法，其特征在于：具体步骤如下：
(1)将壳聚糖溶于乙酸溶液，磁力搅拌直至完全溶解，同时将原儿茶酸溶于乙醇；
(2)将EDC加入到含有MES缓冲液的反应器中；
(3)将步骤(1)所得的原儿茶酸溶液加入反应器中，立即加入N-羟基琥珀酰亚胺(NHS)并调节溶液pH值，随后置于冰水浴中反应，磁力搅拌；
(4)将步骤(1)所得的壳聚糖溶液加入反应器中，反应；
(5)将步骤(4)所得的反应液装入透析袋中，先用自来水透析，再用去离子水透析；
(6)将步骤(5)所得的透析液冷冻干燥后即得壳聚糖-原儿茶酸接枝共聚物；
(7)将步骤(6)所得的接枝共聚物配成水溶液，涂抹于食用菌表面。
3.如权利要求2所述的用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法，其特征在于：步骤(3)中，溶液pH值为5.5，反应时间为1h。
4.如权利要求2所述的用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法，其特征在于：步骤(4)中，在20℃下反应12h。
5.如权利要求2所述的用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法，其特征在于：所述壳聚糖的浓度为5g/L，原儿茶酸的浓度为11.6g/L，EDC的浓度为43g/L，NHS的浓度为8.6g/L。
6.如权利要求2所述的用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法，其特征在于：步骤(7)中，接枝共聚物涂膜液的浓度为10g/L。
7.如权利要求1或2所述的用于食用菌保鲜的酚酸改性壳聚糖涂膜液的制备方法，其特征在于：所述食用菌为杏鲍菇。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109679123A (zh) * | 2018-12-27 | 2019-04-26 | 青岛农业大学 | 一种双交联壳聚糖膜的制备方法 |
| CN111793146A (zh) * | 2020-07-15 | 2020-10-20 | 大连理工大学 | 一种pH敏感型PCA-g-CMCS聚合物及其水凝胶的制备方法 |
| CN111995800A (zh) * | 2020-09-03 | 2020-11-27 | 蔡营龙 | 一种纤维素基抗菌食品包装膜的制备方法 |
| CN114181327A (zh) * | 2021-12-16 | 2022-03-15 | 四川大学 | 一种水溶性改性壳聚糖及其制备方法、应用 |
| CN114933728A (zh) * | 2022-07-01 | 2022-08-23 | 厦门理工学院 | 一种聚乳酸活性多层复合薄膜及其制备方法与应用 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371127A (zh) * | 2014-11-28 | 2015-02-25 | 南京林业大学 | 一种多水分食品包装用的可降解壳聚糖薄膜的制备方法 |
| CN104877047A (zh) * | 2014-12-18 | 2015-09-02 | 扬州大学 | 一种具有强抗氧化活性菊糖-儿茶素接枝共聚物的合成方法 |
-
2016
- 2016-01-15 CN CN201610029415.0A patent/CN106977622A/zh active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371127A (zh) * | 2014-11-28 | 2015-02-25 | 南京林业大学 | 一种多水分食品包装用的可降解壳聚糖薄膜的制备方法 |
| CN104877047A (zh) * | 2014-12-18 | 2015-09-02 | 扬州大学 | 一种具有强抗氧化活性菊糖-儿茶素接枝共聚物的合成方法 |
Non-Patent Citations (2)
| Title |
|---|
| 孔芳等: "壳聚糖复合涂膜对杏鲍菇保鲜效果的研究", 《中国农学学报》 * |
| 苑兆和主编: "《中国果树科学与实践.石榴》", 30 June 2015, 陕西新华出版传媒基团、陕西科学技术出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109679123A (zh) * | 2018-12-27 | 2019-04-26 | 青岛农业大学 | 一种双交联壳聚糖膜的制备方法 |
| CN111793146A (zh) * | 2020-07-15 | 2020-10-20 | 大连理工大学 | 一种pH敏感型PCA-g-CMCS聚合物及其水凝胶的制备方法 |
| CN111793146B (zh) * | 2020-07-15 | 2022-02-11 | 大连理工大学 | 一种pH敏感型PCA-g-CMCS聚合物及其水凝胶的制备方法 |
| CN111995800A (zh) * | 2020-09-03 | 2020-11-27 | 蔡营龙 | 一种纤维素基抗菌食品包装膜的制备方法 |
| CN114181327A (zh) * | 2021-12-16 | 2022-03-15 | 四川大学 | 一种水溶性改性壳聚糖及其制备方法、应用 |
| CN114933728A (zh) * | 2022-07-01 | 2022-08-23 | 厦门理工学院 | 一种聚乳酸活性多层复合薄膜及其制备方法与应用 |
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