天然棕色棉色素的液相色谱组分特性及其指纹图谱分析

发布时间：2018-04-10 18:02

本文选题：天然棕色棉 + 色素　；参考：《浙江理工大学》2017年硕士论文

【摘要】：天然棕色棉被誉为绿色纺织材料,在种植过程中,少需甚至不需喷施农药,污染少;加工过程中不需要染色,既降低了加工成本,又具有生态环保优势,因此具有良好的市场潜力。天然棕色棉的品种繁多,颜色深浅不一,有深棕、浅棕色等。加之天然棕色棉易于被合成染料染色的染色棉假冒,这些都给天然棕色棉制品的检测、鉴别带来了挑战。鉴于天然棕色棉品种的复杂性,研究各品种、各类纺织加工处理后天然棕色棉纤维的色素组分的差异,构建相关的指纹图谱十分必要。本课题分析了全国主要品种的天然棕色棉的色素组成,以及各种处理对天然棕色棉色素组分的影响,并尝试构建各品种、各种处理后的天然棕色棉的色素的液相色谱指纹图谱。具体的研究结论如下:(1)在不同超声条件(时间、温度、料液比)下提取棕色棉色素,采用高效液相色谱(HPLC)对提取液进行分析。结果显示,保留时间前5 min的强极性组分受超声提取条件的影响较大,表现为该保留时间段的色谱峰数量和峰面积的变化较大。比如短时间、低温、高料液比的提取条件得不到1.9 min的组分。温度低于45℃时无法提取到2.5 min的组分,而能够提取到的1.4 min、2.7 min和3.5 min组分的含量较少。保留时间7-20 min的色素物质受提取条件的影响较小,仅表现为不同提取条件下的提取效率不同。这说明,超声条件对提取到的色素组分的组成有明显的影响。以HPLC图中色素各组分的色谱峰数量的多少和峰面积的大小为判断标准,确定了提取到最多组分和最高含量的棕色棉色素的超声条件,即超声时间为4 h、超声温度为55℃、料液比为1:50(g/mL)。(2)收集不同产地、不同品种的天然棕色棉,对其色素提取物的HPLC图谱进行了研究,发现不同品种的天然棕色棉色素的组分相似,但含量具有一定的差异,纤维颜色越接近差异越小,和产地的相关性不明显。不同品种的天然棕色棉色素的HPLC图谱比较相似,保留时间7-20 min的色谱峰基本一致,可认定为天然棕色棉色素的HPLC特征峰。各品种的天然棕色棉中,浅色品种的天然棕色棉的HPLC图谱高度相似,有4个共有峰,保留时间分别为:1.4 min、1.9 min、2.5 min和7-20 min。对各天然浅棕色棉的色素水提取物构建出了高度相关的HPLC指纹图谱;但是,由于深棕和浅棕色棉的色素提取物的HPLC谱图差异较大,其谱图相关性不高,对包括深棕和浅棕在内的各品种棕色棉构建的HPLC指纹图谱不能满足需要。(3)棕色棉纤维经日晒、水洗、高温和煮练处理后,色素各组分的HPLC色谱峰的相对面积都有减小,但程度不同,说明色素各组分的稳定性有所差异。保留时间1.4 min、2.5 min、2.7 min和7-20 min的组分保留时间相对稳定,只是色谱峰面积有不同程度的减小。其中,7-20 min的组分仍然可以作为天然棕色棉(无论经过日晒、水洗、高温和煮练处理与否)的HPLC特征峰。但是,1.9 min和3.5 min的组分不是很稳定,其色谱峰面积变化较大,会逐渐消失。棕色棉纤维经氧化处理后,其色素提取物的HPLC图中只存在2.5min组分的色谱峰,说明氧化处理后大部分色素提取物的结构发生了改变,只有2.5 min组分的结构较稳定,不易被氧化。另外,在日晒、水洗、高温、煮练处理后纤维仍呈棕色,只是颜色深浅发生了变化。但是,氧化后的纤维完全褪色,纤维呈白色,且其提取物的HPLC图中7-20 min的色谱峰消失,说明该色谱峰对应的色素组分是棕色棉色素的主要成分,对棕色棉纤维颜色的呈现起主要作用。日晒、水洗、高温和煮练处理后的棕色棉色素提取物的HPLC图谱差别较大,无法对这些样品建立起相关性较高的指纹图谱。
[Abstract]:The natural brown quilt as a kind of green textile materials, in the planting process, less or no pesticide spraying, less pollution; processing is not needed in the process of dyeing, not only reduces the processing cost, but also has ecological and environmental advantages, so it has good market potential. The natural brown cotton variety, color shades, dark brown in addition, light brown. Natural brown cotton is synthetic dyes dyed cotton fake, which gave the natural brown cotton products detection, identification challenges. Because of the complexity of natural brown cotton varieties, all varieties studied, the difference of all kinds of textile processing pigments in natural brown cotton fiber is separated, it is necessary to the construction of fingerprints related. This paper analyzes the main varieties of natural brown cotton pigment composition, and various effects on the pigment of natural brown cotton group, and try to build various varieties, After various processing of natural brown cotton pigment liquid chromatographic fingerprint. The conclusions are as follows: (1) in different ultrasonic conditions (time, temperature, ratio of material to liquid) under the extraction of brown cotton pigment by high performance liquid chromatography (HPLC) analysis of the extract. The results showed that the retention time before 5 min strong polar components by ultrasonic extraction conditions affect the performance for the changes in the number and peak peak of the reserve time area greatly. Such as the short time, low temperature, high extraction ratio of material to liquid into the 1.9 min component. When the temperature is below 45 DEG C can not be extracted to 2.5 the Min component, and can extract 1.4 min, 2.7 min and 3.5 min less content components. The pigment retention time of 7-20 min was less affected by the extraction conditions, showed only the extraction efficiency of different extraction conditions under different conditions. This shows that the ultrasonic extraction of the pigment There are obvious effects of components. The number of peaks in the HPLC graph of each component of the pigment and the peak area size as a standard, to determine the extraction conditions of ultrasonic most components and the highest content of brown cotton pigment, ultrasonic time was 4 h, ultrasonic temperature is 55 DEG C, liquid is 1:50 (g/mL). (2) collected from different areas, different varieties of natural brown cotton, pigment extract on the HPLC map was studied, found that the pigment of natural brown cotton varieties were similar, but the content is different, more close to the fiber color difference is small, and the origin of the correlation the HPLC map is not obvious. The pigment of natural brown cotton varieties were similar, peak retention time of 7-20 min are basically the same, can be identified as the HPLC characteristic peak of the pigment of natural brown cotton. All varieties of natural brown cotton, light colored varieties of natural brown cotton HPLC was highly similar, there are 4 peaks with retention time were 1.4 min, 1.9 min, 2.5 min and 7-20 min. of the natural light brown cotton pigment aqueous extract to construct HPLC fingerprint highly correlated; however, the pigment extracts from dark brown and light brown cotton HPLC spectra large differences, the spectrum correlation is not high, not on the HPLC fingerprint of different varieties of brown cotton including dark brown and light brown, constructed to meet the needs. (3) brown cotton fiber by the sun, water, and high temperature scouring, HPLC peak pigment components of the area are reduced, but to a different degree, this shows that the stability of pigment components were different. The retention time of 1.4 min, 2.5 min, 2.7 min and 7-20 min component retention time is relatively stable, but the peak area decreased. Among them, 7-20 min components still can be used as a natural brown cotton ( Regardless of the sun, water, and high temperature scouring or not) the characteristic peak of HPLC. However, 1.9 min and 3.5 min component is not very stable, the peak area varies greatly and will gradually disappear. Brown cotton fiber after oxidization, the chromatographic peak of 2.5min components only exist the pigment extract figure HPLC shows that, after oxidation treatment changed the structure of most pigment extract, only 2.5 min components of the structure is stable, not easy to be oxidized. In addition, in the sun, water, high temperature, scouring the treated fiber is brown, but the color depth changed. However, the oxidized fiber completely fade, fibers are white, and the peak of the extracts in the HPLC graph of 7-20 min disappeared, that pigment group of the corresponding chromatographic peak points is the main component of brown cotton pigment, color of brown cotton fiber has played a major role. The sun, water, and high temperature scouring The HPLC Atlas of the brown pigment extracts of the treated brown cotton was very different, and the high correlation fingerprint of these samples could not be established.

【学位授予单位】：浙江理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TS102.211;O657.72

【参考文献】