壳聚糖/明胶抗菌微胶囊的制备及其应用

doi:10.16085/j.issn.1000-6613.2019-1033

摘要/Abstract

摘要：

为了制备用于棉织物天然抗菌整理剂，以绿苋、龙葵和黄柏的复配提取物为芯材，壳聚糖-明胶为壁材，采用复凝聚法制备抗菌微胶囊。研究了乳化剂含量、剪切速度、pH对微胶囊的外观形态及尺寸的影响；借助扫描电子显微镜、傅里叶红外光谱仪等对样品进行表征；将抗菌微胶囊用于棉织物的整理并测试其抗菌性能。结果表明：初乳中乳化剂质量分数为5%、剪切速度为8000r/min、pH为5.7为最佳制备条件，制得的微胶囊尺寸分布在1480～3580nm且热稳定性良好；当微胶囊质量浓度为25g/L，黏合剂质量分数为5%，热烘温度为40℃，整理试样对金黄色葡萄球菌和大肠杆菌的抑菌率分别为89.30%和81.43%，且抑菌效果持久。

关键词: 复凝聚法, 壳聚糖, 棉织物, 抗菌微胶囊, 性能

Abstract:

In order to prepare natural antibacterial finishing agent for cotton fabric, the antibacterial microcapsules were prepared by complex coagulation with compound extract of amaranth, sunflower and cypress as core material and chitosan-gelatin as wall material. The effects of emulsifier content, shear speed and pH on the appearance morphology and size of microcapsules were studied. The samples were characterized by scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FTIR). The antibacterial microcapsules were used in the finishing of cotton fabric and its antibacterial properties were tested. The results showed that the optimum preparation conditions were as follows: the mass fraction of emulsifier in colostrum was 5%, the shear rate was 8000r/min, and the pH was 5.7; the prepared microcapsules had a size distribution between 1480nm and 3580nm and good thermal stability; when the mass concentration of microcapsule was 25g/L, the mass fraction of adhesive was 5% and the hot drying temperature was 40℃, the bacteriostatic rate of the finished sample against Staphylococcus aureus andEscherichia coli was 89.30% and 81.43%, respectively, and the bacteriostatic effect was lasting.

Key words: complex coagulation method, chitosan, cotton fabric, antibacterial microcapsule, properties

中图分类号:

TS195

郑云龙,王进美,孙正琪,秦智成,周娅楠. 壳聚糖/明胶抗菌微胶囊的制备及其应用[J]. 化工进展, 2020, 39(3): 1137-1144.

Yunlong ZHENG,Jinmei WANG,Zhengqi SUN,Zhicheng QIN,Yanan ZHOU. Preparation and application of chitosan/gelatin antibacterial microcapsule[J]. Chemical Industry and Engineering Progress, 2020, 39(3): 1137-1144.

图/表 16

参考文献 24

1	梅林,袁英,李随丽,等.中药血清药理学研究金银花的抑菌活性[J].广州化学,2007(2):31-35.
	MEI Lin,YUAN Ying,LI Suili,et al.Antibacterial activities of flos lonicerae investigated by the means of TCM-Serum pharmaceutical[J].Guangzhou Chemistry,2007(2):31-35.
2	田丁,史梦琪,王赟.连翘挥发油化学成分及其药理作用研究进展[J].天然产物研究与开发,2018,30(10):1834-1842.
	TIAN Ding,SHI Mengqi,WANG Yun.Volatile oil from forsythia suspense: chemical constituents and pharmacological effects[J].Nat. Prod. Res. Dev.,2018,30(10):1834-1842.
3	张晨曦,刘素香,赵艳敏,等.基于液质联用技术的连翘化学成分分析[J].中草药,2016,47(12):2053-2060.
	ZHANG Chenxi,LIU Suxiang,ZHAO Yanmin,et al.Analysis on chemical constituents from Forsythiae Fructus by HPLC-Q-TOF-MS[J].Chinese Traditional and Herbal Drugs,2016,47(12):2053-2060.
4	李梦晓,徐云龙,程晓静,等.茶树油和壳聚糖复合体系的抗菌性能研究[J].材料导报,2015,29(s2):406-408, 417.
	LI Mengxiao,XU Yunlong,CHENG Xiaojing,et al.Antibacterial activity of tea tree oil and chitosan composite system[J].Materials Reports,2015,29(s2):406-408, 417.
5	王亚,黄菁菁,张如全.艾蒿油-壳聚糖抗菌微胶囊的制备及其应用[J].纺织学报,2018,39(10):99-103.
	WANG Ya,HUANG Jingjing,ZHANG Ruquan.Preparation and application of antimicrobial mug wort oil-chitosan microcapsules[J].Journal of Textile Research,2018,39(10):99-103.
6	杨隽颖,吴国祥,陈东梅.苏木植物染料对真丝针织内衣染色抗菌性能及设计要素[J].丝绸,2018,55(7):21-27.
	YANG Junying,WU Guoxiang,CHEN Dongmei.Study on dyeing, antibacterial properties and design elements of silk knitted underwear with hematoxylin plant dyes[J].Journal of Silk,2018,55(7):21-27.
7	周谨.天然植物染料染色与抗菌整理一浴的研究进展[J].针织工业,2016(8):60-63.
	ZHOU Jin.Application pogress of dyeing and antibacterial finishing of natural plant dyes[J].Knitting Industries,2016(8):60-63.
8	苏毅.复合型植物源防紫外整理剂的开发[J].印染助剂,2017,34(6):35-40.
	SU Yi.Development of compound natural plants′UV protective finishing agent[J].Textile Auxiliaries,2017,34(6):35-40.
9	KUMAR A,LAKSHMAN K,JAYAVEERA K,et al.Estimation of Rutin and Quercetin in Amaranthus viridis Linn by HPLC[J].Asian J. Exp. Sci.,2009,23(1):51-54.
10	LAKO J,TRENERRY VC,WAHLQVIST M,et al.Phytochemical flavonols, carotenoids and the antioxidant properties of a wide selection of Fijian fruit, vegetables and other readily available foods[J].Food Chemistry,2007,101(4):1727-1741.
11	KOSALEC I,BAKMAZ M,PEPELJNJAK S,et al.Quantitative analysis of the flavonoids in raw propolis from northern Croatia[J].Acta Pharmaceutica,2004,54(1):65-72.
12	GHASEMZADEH A,JAAFAR HZ,RAHMAT A.Antioxidant activities, total phenolics and flavonoids content in two varieties of Malaysia young ginger (Zingiber officinale Roscoe)[J].Molecules,2010,15(6):4324-4333.
13	车秋凌,李明春,辛梅华.壳聚糖及其衍生物在天然织物整理中的应用研究进展[J].化工进展,2018,37(11):4330-4336.
	CHE Qiuling,LI Mingchun,XIN Meihua.Research progress of chitosan and its derivatives in natural fabric finishing[J].Chemical Industry and Engineering Progress,2018,37(11):4330-4336.
14	何日安,岳武,姚评佳,等.低分子量壳聚糖对植物病原菌的抑制作用研究[J].安徽农业科学,2009,37(4):1566-1568.
	HE Ri’an,YUE Wu,YAO Pingjia,et al.Study on inhibiting effect of low molecular weight chitosans on plant pathogenic bacteria[J].Journal of Anhui Agricultural Sciences,2009,37(4):1566-1568.
15	吕海宁.壳聚糖在纺织品功能整理方面的应用[J].印染助剂,2015,32(12):1-6.
	Haining LÜ.Application of chitosan in functional finishing of textiles[J].Textile Auxiliaries,2015,32(12):1-6.
16	ZHANG X,LIU Y P,YONG H M,et al.Development of multifunctional food packaging films based onchitosan, TiO₂ nanoparticles and anthocyanin-rich black plum peel extract[J].Food Hydrocolloids,2019,94:80-92.
17	WIJESIRIGUNAWARDANA P B,PERER B G K.Development of a cotton smart textile with medicinal properties using lime oil microcapsules[J].Acta Chimica Slovenica,2018,65(1):150-159.
18	MOSCHONA A,LIAKOPOULOU-KYRIAKIDES M.Encapsulation of biological active phenolic compounds extracted from wine wastes in alginate-chitosan microbeads[J].Journal of Microencapsulation,2018,35(3):229-240.
19	HU J,ZhANG Y D,XIAO Z B,et al.Preparation and properties of cinnamon-thyme-ginger composite essential oil nanocapsules[J].Industrial Crops and Products,2018,122:85-92.
20	尹文萱,王兴涌,王建怀,等.芦丁和槲皮素及其金属配合物的FTIR研究[J].中国矿业大学学报,2009,38(6):884-888.
	YIN Wenxuan,WANG Xingyong,WANG Jianhuai,et al.FTIR study of Rutin, Quercetin and their metal complexes[J].Journal of China University of Mining & Technology,2009,38(6):884-888.
21	宗水珍.苦黄注射液中乙酸乙酯萃取物成分表征[J].理化检验(化学分册),2000(12):547-548, 550.
	ZONG Shuizhen.The characterization of components in the ethyl acetate extract of the Kuhuang injection[J].Physical Testing and Chemical Analysis(Part B: Chemical Analysis),2000(12):547-548, 550.
22	蔡卫家,徐显贵.黄柏药材的红外光谱鉴别[J].中国药业,2011,20(20):34.
	CAI Weijia,XU Xiangui.Identification of phellodendron chinense by infrared spectroscopy[J].China Pharmaceuticals,2011,20(20):34.
23	蒋柳云,李玉宝,张利,等.纳米羟基磷灰石/壳聚糖/羧甲基纤维素三元复合骨修复材料的制备和性能研究[J].功能材料,2007(5):798-801.
	JIANG Liuyun,LI Baoyu,ZHANG Li,et al.Preparation and characterization of nano-hydroxyapatite /chitosan /carboxymethyl cellulosecomposite used for bone repair[J].Journal of Functional Materials,2007(5):798-801.
24	沈萍，陈向东.微生物学[M].北京:高等教育出版社,2006:72-76.
	SHEN Ping,CHEN Xiangdong.Microbiology[M].Beijing:Higher Education Press,2006:72-76.

名称	规格	生产厂家
绿苋	—	市售
龙葵、黄柏	—	国药控股陕西大药房
纯棉织物	133.2g/m²	宏达织布厂
明胶	AR	天津市天力化学试剂有限公司
无水乙醇	AR	天津市大茂化学试剂厂
壳聚糖	脱乙酰度＞95%	上海阿拉丁生化科技股份有限公司
冰乙酸	AR	天津市富宇精细化工有限公司
戊二醛	AR	天津市福晨化学试剂厂
氢氧化钠	AR	天津市天力化学试剂有限公司
司班-20	非离子型	江苏省海安石油化工厂
水性聚氨酯	—	上海伊纯实业有限公司
琼脂粉	BR	北京奥博星生物技术有限责任公司
牛肉膏	BR	北京奥博星生物技术有限责任公司
蛋白胨	BR	北京奥博星生物技术有限责任公司
磷酸氢二钠	AR	天津市科密欧化学试剂有限公司
磷酸二氢钾	AR	天津市大茂化学试剂厂
氯化钠	AR	天津市大茂化学试剂厂
氢氧化钠	AR	洛阳昊华化学试剂有限公司

名称	规格	生产厂家
绿苋	—	市售
龙葵、黄柏	—	国药控股陕西大药房
纯棉织物	133.2g/m²	宏达织布厂
明胶	AR	天津市天力化学试剂有限公司
无水乙醇	AR	天津市大茂化学试剂厂
壳聚糖	脱乙酰度＞95%	上海阿拉丁生化科技股份有限公司
冰乙酸	AR	天津市富宇精细化工有限公司
戊二醛	AR	天津市福晨化学试剂厂
氢氧化钠	AR	天津市天力化学试剂有限公司
司班-20	非离子型	江苏省海安石油化工厂
水性聚氨酯	—	上海伊纯实业有限公司
琼脂粉	BR	北京奥博星生物技术有限责任公司
牛肉膏	BR	北京奥博星生物技术有限责任公司
蛋白胨	BR	北京奥博星生物技术有限责任公司
磷酸氢二钠	AR	天津市科密欧化学试剂有限公司
磷酸二氢钾	AR	天津市大茂化学试剂厂
氯化钠	AR	天津市大茂化学试剂厂
氢氧化钠	AR	洛阳昊华化学试剂有限公司

名称	型号	生产厂家
弗鲁克高剪切分散乳化机	FA25	上海右一仪器有限公司
恒温摇床	TS-1102C	上海天呈实验企业制造有限公司
光照摇床	TS-211GZ	上海天呈实验企业制造有限公司
光照培养箱	GZX-150BS-Ⅲ	上海新苗医疗器械制造有限公司
手提式压力蒸汽灭菌器	DSX-280B	上海申安医疗器械厂
干燥灭菌箱	GX-65B	天津市泰斯特仪器有限公司
快速混匀器	SK-1	常州赛普实验仪器厂
超净工作台	SW-CJ-1FD	苏州净化设备有限公司
气流烘干器	C型	郑州汇成科工贸有限公司
旋转蒸发器	RE52-98	上海亚荣生化仪器厂
索氏提取器	—	北京启文海龙玻璃制品有限公司

名称	型号	生产厂家
弗鲁克高剪切分散乳化机	FA25	上海右一仪器有限公司
恒温摇床	TS-1102C	上海天呈实验企业制造有限公司
光照摇床	TS-211GZ	上海天呈实验企业制造有限公司
光照培养箱	GZX-150BS-Ⅲ	上海新苗医疗器械制造有限公司
手提式压力蒸汽灭菌器	DSX-280B	上海申安医疗器械厂
干燥灭菌箱	GX-65B	天津市泰斯特仪器有限公司
快速混匀器	SK-1	常州赛普实验仪器厂
超净工作台	SW-CJ-1FD	苏州净化设备有限公司
气流烘干器	C型	郑州汇成科工贸有限公司
旋转蒸发器	RE52-98	上海亚荣生化仪器厂
索氏提取器	—	北京启文海龙玻璃制品有限公司

抗菌级别	水洗次数	抑菌率/%
抗菌级别	水洗次数	金黄色葡萄球菌	大肠杆菌	白色念珠菌
A级	10	≥99	不考核	不考核
AA级	20	≥80	≥70	≥60
AA级	50	≥80	≥70	≥60