CN108249420B - 一种带正电的碳点及其制备方法和应用 - Google Patents
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Abstract
本发明公开了一种带正电的碳点，以聚赖氨酸为碳源制备得到。其制备包括：称取一定量的聚赖氨酸，用适量去离子水溶解，将混匀的聚赖氨酸水溶液置于微波场中加热，反应结束经冷却后加入适量去离子水，超声处理一段时间，离心，收集碳点水溶液经超微膜透析，再经冷冻干燥后制成所述的带正电的碳点粉末。还公开了所述的带正电的碳点在食品抑菌中的应用。本发明制备工艺简单，产物纯度高，反应时间短，碳点尺寸可控，制备得到的具有超富正电碳点可用来抑制食品中的腐败微生物，选择性高，在食品安全及荧光复合材料等方面有重大意义和广泛的应用前景。
Description
技术领域
本发明涉及一种纳米材料的制备方法，具体涉及一种带正电的碳点及其制备方法和应用。
背景技术
近年来，各种各样有关碳点的研究引起了人们的广泛关注。碳纳米材料由于具有良好的生物相容性及原料廉价易得的优点，使其被广泛应用于生物检测、催化、能源、电子器件以及载药等方面，但是目前为止有碳点用于抗菌方面的报道较少，更未见有关其在食品贮藏与保鲜方面的应用研究报道。
聚赖氨酸(ε-PL)是赖氨酸的α位羰基和β位氨基结合的聚物。小鼠试验证实，聚赖氨酸不会对生殖、神经和免疫器官、胚胎和胎儿生长产生毒性。日本已批准ε-PL作为防腐剂添加于食品中。聚赖氨酸的抑菌谱很广，对革兰氏阳性菌、革兰氏阴性菌、酵母、霉菌的生长都有抑制作用，对细菌的抑菌效果最佳，其次为酵母菌和霉菌。细菌对聚赖氨酸的敏感性较强，最小抑菌浓度都不高于25mg/L；而真菌的最小抑菌浓度较高，尤其是霉菌。聚赖氨酸能耐高温，加热后抑菌效果基本不受影响。pH对聚赖氨酸的抑菌性有一定影响，pH为7的抑菌效果较好，抑菌时间比较长；pH为5达到最佳抑菌效果最快，但保持时间不长；在过酸或过碱的条件下抑菌效果不是很好，尤其是在碱性条件下。
聚赖氨酸，由于其表面带正电荷，可以以静电吸附的方式与带负电的细菌表面相结合，带有正电荷的季铵基亲水头部可取代细菌表面对细胞膜具有稳定作用的Mg2+、Ca2+，引起细菌膜渗透性调节功能的丧失以及钾离子和质子的外泄。此外，具有疏水长碳烷烃链的季铵盐衍生物可以穿透细菌的胞壁，与细胞膜中的磷脂双分子层和膜蛋白发生作用，通过扰动细菌细胞膜磷脂双分子层的稳定状态，从而引起细胞膜溶解、内容物泄漏和细菌死亡。这类通过作用于细菌细胞壁/细胞膜而产生抗菌效果的抗菌试剂可以有效避免细菌产生耐药性，因此季铵盐类抗菌剂具有十分广阔的应用前景。
目前，在用有机碳源制备碳点时主要采用自下而上法，其中最常用的有干热法。但这些方法都存在产率低、成本高、制备工艺复杂、制备的碳点尺寸可控性差等问题。因此，寻求产率高、低成本、简单易行的新的制备碳点的方法，是进一步有效利用以及拓展碳点应用的必经之路。
发明内容
本发明目的在于解决现有技术中的不足之处，提供了一种带正电的碳点及其制备方法和应用，本发明方法操作简单，得到的碳点尺寸可控，在食品抑菌中有广泛应用。
本发明采用的技术方案如下：
一种带正电的碳点，以聚赖氨酸为碳源制备得到。
所述碳点的平均粒径为2～10nm，激发波长320～440nm，依赖于激发波长的发射波长在400～460nm。
所述碳点在270nm附近具有最强的紫外吸收峰；且具有荧光特性，最大激发波长为365nm，最大发生波长为445nm左右。
所述碳点为富正电的碳点，所述碳点的ZETA电位为+40～+50mV。
本发明还提供了一种所述的带正电的碳点的制备方法，包括：称取一定量的聚赖氨酸，用适量去离子水溶解，将混匀的聚赖氨酸水溶液置于微波场中加热，反应结束经冷却后加入适量去离子水，超声处理一段时间，离心，收集碳点水溶液经超微膜透析，再经冷冻干燥后制成所述的带正电的碳点粉末。
本发明利用微波辅湿热法合成碳点，相比于常规的热传递模式，微波加热均匀，速度快且没有加热滞后性及温度梯度；微波辐射还起到催化剂的作用，改变了反应的动力学，降低了反应活化能，提高反应速率。
其中，每克聚赖氨酸溶解于5～10mL去离子水中。
所述微波场的辐射功率为700～1500W，加热时间为5～25min。
所述超声处理的功率为150～200w，处理时间为40～60min。
将反应后的混合溶液通过离心除去不溶性沉淀及大颗粒聚集体，离心转速为8000～20000rpm/min，离心时间为30～60min。
所述超微膜的孔径为0.20～0.25μm，透析时间为1～3天。
本发明采用冷冻干燥收集碳点粉末，较大程度上地解决了碳点产率低的问题。
本发明的另一目的是提供一种所述的带正电的碳点在食品抑菌中的应用，所述的碳点用于制备食品保鲜剂或者抑菌剂。具有超富正电的碳点表面含有丰富的正电荷，能以静电吸附的方式与带负电的细菌表面相结合，取代细菌表面对细胞膜具有稳定作用的Mg2+、Ca2+，引起细菌膜渗透性调节功能的丧失以及钾离子和质子的外泄。对常见的食源性致病菌(如单增李斯特菌、大肠杆菌、金黄色葡萄球菌、枯草芽孢杆菌等)都表现出较强的抑制作用，可单独或与其它食品防腐剂或抑菌剂复配，广泛应用于食品贮藏与保鲜领域。
与现有技术相比，本发明具有如下有益效果：
(1)本发明利用微波湿热法，以聚赖氨酸为碳源制备具有超富正电荧光碳点，制备工艺简单，产物纯度高，反应时间短；本发明制备的具有超富正电碳点尺寸可控。
(2)通过该合成方法制备具有超富正电碳点，所得具有超富正电碳点可用来抑制食品中的腐败微生物，选择性高，在食品安全、生物成像及荧光复合材料等方面有重大意义和广泛的应用前景。
附图说明
图1为实施例1制备的碳点的紫外吸收光谱；
图2为实施例1制备的碳点的荧光发射光谱(激发波长为365nm)；
图3为实施例1制备的碳点的TEM图；
图4为对比例1与实施例1制得的碳点对S.aureus与E.coli的MIC；
图5为对比例1与实施例1制得的碳点对S.aureus与E.coli的MBC。
具体实施方式
下面结合具体实施例，进一步阐明本发明，但本发明不限于此。
实施例1
微波湿热法制备碳点：
称取1g聚赖氨酸，溶于6mL去离子水中超声搅拌。将混匀的聚赖氨酸水溶液置于圆底烧瓶中，将其置于微波场中加热7～10min，充分反应后，停止加热，自然冷却至室温。将上述液体溶于5mL去离子水中，超声场中作用一段时间，使全部所得碳点溶于水中；离心分离，除去不溶性沉淀和大粒径聚集体，澄清碳点水溶液经0.25μm的超微膜透析，得到淡黄色澄清透明的溶液，将澄清碳点溶液置于冷冻干燥仪中，经冷冻干燥后制成碳点粉末，收集碳点粉末至于4℃保存备用，收率为40％。
其中，所述微波场的辐射功率为800W，加热时间为8min；超声处理的功率为180W，处理时间为60min；离心转速为20000rpm/min，离心时间为60min。
经测定，所得碳点的ZETA电位为+46mV。
对比例1
本对比例探究以聚赖氨酸为起始原料，利用常规耗时干热法与微波湿热法制备的碳点差异，比较两种条件下碳点的荧光表征、粒径大小及抑菌能力。
常规干热法制备碳点：
称取1g聚赖氨酸，置于10mL干净的坩埚中，将其至于马弗炉中，升高温度至270℃，继续加热2h，充分反应后，停止加热，自然冷却至室温。向坩埚中加入5mL去离子水，并置于超声场中作用一段时间，使全部所得碳点溶于水中；离心分离，除去不溶性沉淀和大粒径聚集体，澄清碳点水溶液经0.25μm的超微膜透析，得到淡黄色澄清透明的溶液，将澄清碳点溶液置于冷冻干燥仪中，经冷冻干燥后制成碳点粉末，收集碳点粉末至于4℃保存备用，收率为20％。
其中，超声处理的功率为180W，处理时间为60min；离心转速为20000rpm/min，离心时间为60min。
图1为实施例1微波湿热法制备的碳点的紫外吸收光谱图，图2为实施例1微波湿热法制备的碳点的荧光发射光谱(激发波长为365nm)，如图1～2所示，实施例1微波湿热法所得碳点的最大紫外吸收峰在270nm，在365nm的激发波长下，最大发射波长为445nm左右。粒径分布结果表明微波湿热法所得碳点粒径大小为2～10nm，而对比例1常规干热法所得碳点粒径大小为5～15nm。并对碳点的形貌等进行了透射电子显微镜TEM表征，如图3所示，表明在微波湿热法合成的碳点分散性好，且较为均匀。
实施例2
微波湿热法制备碳点：
称取1g聚赖氨酸，溶于6mL去离子水中超声搅拌。将混匀的聚赖氨酸水溶液置于圆底烧瓶中，将其置于微波场中加热7～10min，充分反应后，停止加热，自然冷却至室温。将上述液体溶于5mL去离子水中，超声场中作用一段时间，使全部所得碳点溶于水中；离心分离，除去不溶性沉淀和大粒径聚集体，澄清碳点水溶液经0.25μm的超微膜透析，得到淡黄色澄清透明的溶液，将澄清碳点溶液置于冷冻干燥仪中，经冷冻干燥后制成碳点粉末，收集碳点粉末至于4℃保存备用，收率约为42％左右。
其中，所述微波场的辐射功率为700W，加热时间为10min；超声处理的功率为170W，处理时间为50min；离心转速为20000rpm/min，离心时间为60min。
实施例3
微波湿热法制备碳点：
称取1g聚赖氨酸，溶于6mL去离子水中超声搅拌。将混匀的聚赖氨酸水溶液置于圆底烧瓶中，将其置于微波场中加热7～10min，充分反应后，停止加热，自然冷却至室温。将上述液体溶于6mL去离子水中，超声场中作用一段时间，使全部所得碳点溶于水中；离心分离，除去不溶性沉淀和大粒径聚集体，澄清碳点水溶液经0.25μm的超微膜透析，得到淡黄色澄清透明的溶液，将澄清碳点溶液置于冷冻干燥仪中，经冷冻干燥后制成碳点粉末，收集碳点粉末至于4℃保存备用，收率约为33％。
其中，所述微波场的辐射功率为1000W，加热时间为5min；超声处理的功率为160W，处理时间为60min；离心转速为20000rpm/min，离心时间为60min。
应用例1
本应用例探究用常规加热法和微波湿热法制得碳点的抑菌能力的区别。
两种方法制得的碳点由实施例1和对比例1中所述步骤制得。抑菌实验的具体操作如下：
准备60个15mL的试管，8个50ml锥形瓶(每个锥形瓶中装有9mLTSB培养基)、60个培养皿、2瓶装有500mL TSA培养基的1000mL锥形瓶，10个试管一捆，向每个试管中加入9mL生理盐水(氯化钠的质量浓度为0.85％)后盖上试管塞并用4层报纸包住。8个锥形瓶需用8层纱布封口并且每个锥形瓶的纱布外部用4层报纸包住，培养皿也需要用4层报纸包住(10个/包)。121℃灭菌20min后放入105℃烘箱(装有生理盐水的试管与装有TSB培养基的锥形瓶不需要烘干)，烘干1h后。取5ml离心管在天平上分别称取2.5ug两种方法制备的碳点，并用50uL超纯水溶解，制备浓度为50ug/mL的抑菌剂母液。盖上离心管的盖子后置于超声清洗仪中溶解，并放入超净台。对超净台进行20min的紫外灭菌后，用TSA培养基倒60块平板，待其凝固后在超净台中将菌液稀释至107CFU/mL，并分别从中吸取1mL至8个50mL锥形瓶(每个锥形瓶汇总装有9mL的TSA培养基)中使最终菌液浓度保持在106CFU/mL，分别向8个锥形瓶中加入不同体积的抑菌剂母液。将8个锥形瓶用8层纱布封口放入180r/min，37℃的摇床培养24h后对8个锥形瓶进行涂布计数，该实验重复平行三次。
MIC是基于菌液浓度的对数差异(Log DP)。Log DP的定义是根据如下的等式(1)：
Log DP＝Log(N/No)＝Log(N)－Log(N0) (1)
式中，N——培养24h后的菌液浓度；No——原始的菌液浓度。
最小抑菌浓度(MIC)的定义是在一定培养条件下培养24小时，能抑制某种微生物明显增长的最低药物浓度(Log DP≤0)。最小杀菌浓度(MBC)定义为在一定培养条件下培养24小时之后初始菌液浓度的99.9％以上的菌都被杀死的最低药物浓度(Log DP≤-3)。
传统干热法与微波湿热法制得的碳点对S.aureus与E.coli的MIC如图4所示，MBC如图5所示。显然微波湿热法制得具有超富正电碳点的抑菌效果明显优于干热法，其中对金黄色葡萄球菌(S.aureus)的MIC及MBC，普通干热法均为微波湿热法的4倍。而对大肠杆菌(E.coli)的MIC及MBC，普通干热法较微波湿热法分别高出8倍及4倍。
Claims (8)
1.一种带正电的碳点，其特征在于，所述的带正电的碳点的制备方法包括：称取一定量的聚赖氨酸，用适量去离子水溶解，将混匀的聚赖氨酸水溶液置于微波场中加热，反应结束经冷却后加入适量去离子水，超声处理一段时间，离心，收集碳点水溶液经超微膜透析，再经冷冻干燥后制成；
所述微波场的辐射功率为700～1500W，加热时间为5～25min。
2.根据权利要求1所述的带正电的碳点，其特征在于，所述碳点的平均粒径为2～10nm，激发波长在320～440nm，依赖于激发波长的发射波长在400～460nm。
3.根据权利要求1所述的带正电的碳点，其特征在于，每克聚赖氨酸溶解于5～10mL去离子水中。
4.根据权利要求1所述的带正电的碳点，其特征在于，所述超声处理的功率为150～200w，处理时间为40～60min。
5.根据权利要求1所述的带正电的碳点，其特征在于，离心转速为8000～20000rpm/min，离心时间为30～60min。
6.根据权利要求1所述的带正电的碳点，其特征在于，所述超微膜的孔径为0.20～0.25μm。
7.一种根据权利要求1所述的带正电的碳点在食品抑菌中的应用。
8.根据权利要求7所述的带正电的碳点在食品抑菌中的应用，其特征在于，所述的碳点用于制备食品保鲜剂或者抑菌剂。
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