摘要
针对进口粗水洗羽毛绒监管中存在的鉴别难题,建立未水洗与粗水洗羽毛绒的快速检测方法,采用差示扫描量热法(DSC)为核心检测手段,结合热重分析(TG)、X射线衍射(XRD)及红外光谱分析进行方法验证,选取自然风干及80~160℃热处理的粗水洗羽毛绒样品,系统分析其角蛋白热稳定性、晶体结构及二级结构变化特征,最后通过对比白鸭毛、灰鸭毛及其羽绒制品的DSC曲线差异,建立特征峰识别体系。TG结果显示羽毛绒热分解呈现水分蒸发、角蛋白降解和残余分解三阶段特征;XRD证实热处理引起角蛋白晶体结构重构;红外光谱定量分析表明样品粗水洗后β-折叠结构比例增加,无规卷曲结构减少;DSC检测显示白鸭毛、白鸭绒和灰鸭绒粗水洗样品在170~220℃区间产生明显特征峰。基于DSC曲线特征峰差异,建立了一种快速检测方法,用于区分未水洗与粗水洗羽毛绒,该方法可定性分析80~140℃热处理对羽毛角蛋白结构的影响,为海关监管及行业标准修订提供了技术支撑。
Objective The global trade of substandard feather and down products,particularly those subjected to inadequate washing processes,poses significant challenges to customs inspection and epidemic prevention.Existing standards like GB/T 17685-2016 fail to address the identification of these substandard products,which lack sufficient hygiene and structural stability.This study aimed to establish a rapid,reliable detection method based on differential scanning calorimetry(DSC)to distinguish unwashed and inadequately washed feather and down by characterizing heat-induced keratin conformational changes,thereby providing technical support for regulatory standard revisions.Method Thermogravimetry(TG),X-Ray Diffraction(XRD),Fourier-transform infrared spectroscopy(FT-IR)and differential scanning calorimetry(DSC)were employed to compare the thermal stability of feather and down samples.For sample preparation,unwashed samples(white/grey duck feather and down)were subjected to natural air-drying or heat treatments(80-160℃for 30 min).TG was employed to quantify the mass loss across 30-800℃(10℃/min,N 2 atmosphere)for unwashed and heat-treated(80-160℃,30 min)white/grey duck feather/down.XRD(5°-25°,5(°)/min)and FT-IR(4000-400 cm^(-1),4 cm^(-1) resolution)results were examined to analyze the crystal structure evolution and secondary structural transitions(β-sheet,α-helix,random loops).As the core technique for capturing thermal behavior details,DSC(5℃/min to 550℃,N 2 flow)played a critical role in establishing distinct thermal fingerprints for all 24 sample groups(4 types and 6 treatments),focusing on endothermic peak variations correlated with keratin denaturation.Data were processed using NETZSCH Proteus and Origin 2022,with statistical validation of structural parameters.Results TG analysis revealed three-phase decomposition of feather and down,which are moisture evapora-tion(30-200℃),keratin degradation(200-400℃),and residual decomposition(400-800℃).For structural transitions,XRD revealed that 120℃ treatment increased α-helix and β-sheet diffraction intensity in white feather,while 160℃ reduced α-helix and β-sheet peaks in grey feather.FT-IR deconvolution showed that inadequate washing elevated β-sheet content and eliminated random loops,confirming molecular rearrangement into stable hydrogen-bonded networks.DSC results indicated that unwashed samples exhibited broad moisture evaporation peaks at(83.2-91.7)℃.After heat treatment,peak positions shifted or disappeared.80-140℃ treatments induced distinct β-sheet denaturation peaks within 170-220℃.Specifically,160℃ treatment caused structural disorder,reducing enthalpy and peak broadening.Meanwhile,grey feather displayed similar trends but varied in peak intensity due to structural differences.Conclusion In this study,the thermochemical properties of inadequately washed and unwashed feather/down were investigated through TG,XRD,FT-IR,and DSC analysis.The study concluded that heat treatment is a key factor affecting the thermal properties of down keratin.The DSC results showed that the DSC curves of inadequately washed and unwashed feather/down are different,and unwashed and inadequately washed feather/down can be distinguished by the characteristic peaks on the DSC curves.The DSC method effectively distinguishes unwashed and inadequately washed feather/down based on thermal transition differences.This method requires minimal sample preparation(10 mg)and provides results within 1 h,offering a rapid and reliable solution for customs inspection and quality control.The findings support the revision of GB/T 17685-2016 to include thermal analysis criteria,enhancing the regulation of substandard products in the global down industry.
作者
周小叶
曹爱玲
苏日娜
石文军
赵仙梅
杜达生
蔡路昀
ZHOU Xiaoye;CAO Ailing;SU Rina;SHI Wenjun;ZHAO Xianmei;DU Dasheng;CAI Luyun(Ningbo Global Innovation Center,Zhejiang University,Ningbo,Zhejiang 315100,China;College of Biosystems Engineering and Food Science,Zhejiang University,Hangzhou,Zhejiang 310058,China;Silk Inspection Center of Hangzhou Customs District,Hangzhou,Zhejiang 310007,China;Technology Center of Qingdao Customs,Qingdao,Shandong 266001,China;Zhejiang Liuqiao Industrial Co.,Ltd.,Hangzhou,Zhejiang 311200,China;Zhejiang Samsung Down Co.,Ltd.,Hangzhou,Zhejiang 311200,China)
出处
《纺织学报》
北大核心
2025年第10期46-53,共8页
Journal of Textile Research
基金
国家海关总署科技项目(2022HK106,2024HK306,2023HK077)。
关键词
粗水洗羽毛绒
未水洗羽毛绒
差示扫描热量法
羽毛绒角蛋白结构
羽绒
inadequately washed feather and down
unwashed feather and down
differential scanning calorimetry
keratin structure of feather and down
down
