摘要
利用高效液相色谱,获取不同来源鲜茧和干茧生丝的高效液相色谱图,然后通过特征组分信息的提取,文章分别建立鲜茧/干茧生丝各自的HPLC(高效液相色谱法)指纹图谱,并利用指纹图谱对生丝样品进行相似度评价和系统聚类分析,来验证其对生丝的区分效果。结果表明:鲜茧生丝样品之间相似度大于0.919,干茧生丝样品之间相似度大于0.945,同类生丝的一致性良好。但鲜茧、干茧生丝的指纹谱图存在明显差别,说明两类生丝的特征组分不同。根据两类生丝的特征差异进行系统聚类分析,可以完成对两类生丝的准确区分。经方法学验证,指纹图谱用于鲜茧、干茧生丝定性时具有良好的可靠性和可重复性。鲜茧/干茧生丝HPLC指纹图谱能反映出两类生丝的组分差异,可以作为鲜茧/干茧生丝的区分依据。
Silk has a long history as a textile raw material in China.People usually divide silk into two categories according to the different ways of reeling.The raw silk prepared by cocoon drying and cocoon cooking is called dry cocoon raw silk,and the raw silk obtained by direct reeling only through infiltration is called fresh cocoon raw silk.Due to the different reeling processes,the components of the two kinds of raw silk are different,which makes the cohesion and tensile properties of raw silk different.These differences in the performance of raw silk affect the quality of the final woven silk fabric,so it is necessary to distinguish the two kinds of raw silk.However,since the components of fresh cocoon/dry cocoon raw silk are easily affected by factors such as origin and silkworm eggs,it is difficult to ensure the accuracy of identification.Therefore,in this paper,the HPLC fingerprint of fresh cocoon and dry cocoon raw silk was constructed to realize the accurate distinction between the two kinds of raw silk.In this study,representative raw silk samples from different sources on the market were selected to prepare raw silk extract and perform HPLC detection.The obtained spectrum was imported into the similarity evaluation system for spectrum correction and automatic matching,and the retention time and peak area values of each chromatographic peak were obtained.The average retention time and relative peak area were calculated to complete the calibration of the characteristic peaks.The common pattern fingerprints of the two types of cocoon filaments were determined by the average method,and the similarity value of each raw silk sample was calculated by the cosine value of the angle.By counting the similarity values of similar cocoon filaments,the similarity threshold of similar cocoon filaments is set as the basis for preliminary determination.After that,the fresh cocoon/dry cocoon raw silk samples were subjected to cluster analysis.The inter-group association method was used as the cluster analysis method.The average Euclidean distance was selected as the measurement standard,and the two types of raw silk were distinguished by cluster analysis.According to the experimental results,the RSD of retention time of fresh cocoon raw silk samples is less than 1.17%,and the RSD of relative peak area is in the 20.42%-107.27% range.The RSD of retention time of dried cocoon raw silk is less than 1.36%,and the RSD of relative peak area is in the 4.72%-88.15% range.The components of each raw silk sample are similar,but the content of each component is quite different.The common fingerprint of fresh cocoon and dry cocoon raw silk shows that the fresh cocoon raw silk has a strong peak at the retention time of 1.71 min,a moderate peak at the retention time of 2.02 min,5.87 min,8.69 min and 10.34 min,and there are some weak peaks between the retention time of 14.50 min and 16.50 min.The dry cocoon raw silk shows a strong peak at the retention time of 1.70 min,and there are only two moderate peaks at the retention time of 2.02 min and 5.64 min.The common fingerprints of fresh and dry cocoons are significantly different.The similarity evaluation results show that the similarity threshold of fresh cocoon raw silk is 0.919,and the similarity threshold of dried cocoon raw silk is 0.945.The similarity between the same kind of raw silk is good,and the similarity between dry cocoon raw silk is better than that of fresh cocoon raw silk,which is consistent with the RSD results of relative peak area.The results of cluster analysis show that the two types of raw silk samples could be accurately distinguished when the clustering rescaling distance is 3.The results show that the HPLC fingerprint can show the component information of raw silk more comprehensively and meet the identification requirements of fresh/dry cocoon raw silk.The fresh/dried cocoon raw silk can be identified by HPLC fingerprint.
作者
徐航
马明波
叶飞
杨亚娟
周文龙
XU Hang;MA Mingbo;YE Fei;YANG Yajuan;ZHOU Wenlong(College of Textile Science and Engineering(International Institute of Silk),Zhejiang Sci-Tech University,Hangzhou 310018,China;Huzhou Institute of Quality and Technical Supervision and Inspection(Huzhou Fiber Quality Monitoring Center),Huzhou 313099,China;Wenzhou University of Technology,Wenzhou 325035,China)
出处
《丝绸》
CAS
CSCD
北大核心
2023年第8期21-27,共7页
Journal of Silk
基金
湖州市科技计划项目(2022GZ11)。
关键词
鲜茧生丝
干茧生丝
高效液相色谱
指纹图谱
相似度评价法
聚类分析
fresh cocoon raw silk
dried cocoon raw silk
high performance liquid chromatography
fingerprint
similarity evaluation method
cluster analysis
