热辅助在线衍生化-气相色谱法测定聚3-羟基丁酸-戊酸酯/聚乳酸混合纤维  

Determination of poly(3-hydroxybutyrate-co-hydroxyvalerate)/poly(lactic acid)blend fibers by thermochemolysis-gas chromatography

作　　者：黄忠平 吴尔苗[1] 石东亮 潘保全 林慈慧 郑睿行 沈坚 HUANG Zhongping;WU Ermiao;SHI Dongliang;PAN Baoquan;LIN Cihui;ZHENG Ruixing;SHEN Jian(Ningbo Academy of Product and Food Quality Inspection(Ningbo Fiber Inspection Institute),Ningbo 315048,China;College of Chemical Engineering,Zhejiang University of Technology,Hangzhou 310014,China)

机构地区：[1]宁波市产品食品检验研究院(宁波市纤维检验所),宁波315048 [2]浙江工业大学化学工程学院,杭州310014

出　　处：《分析试验室》2024年第9期1338-1343,共6页Chinese Journal of Analysis Laboratory

基　　金：宁波市自然科学基金项目(2023J197);浙江省基础公益研究计划项目(LGC20B050013)资助。

摘　　要：建立了热辅助在线衍生化-气相色谱法测定混合纤维中聚3-羟基丁酸-戊酸酯/聚乳酸(PHBV/PLA)的含量及比例。采用三氯甲烷溶解纤维样品,四甲基氢氧化铵(TMAH)进行衍生化,PHBV/PLA在高温裂解下瞬间生成甲基化产物,由气相色谱-氢火焰离子化检测器-质谱分离测定。结果表明,PHBV特征甲基化产物在绝对进样量0.075~7.50μg范围内线性关系良好,线性相关系数(r)为0.9954;PLA特征甲基化产物在绝对进样量0.35~17.50μg范围内线性关系良好,r为0.9932。PHBV和PLA特征甲基化产物的定量限分别为0.075μg和0.35μg,相对标准偏差(RSD)分别为6.0%和4.8%,加标回收率分别在100.8%~107.6%和91.3%~104.5%之间。本研究为共混纤维中PHBV/PLA的定性鉴别和定量检测提供了方法参考。A simple and sensitive method based on thermochemolysis-gas chromatography was established and applied to the determination of poly(3-hydroxybutyrate-co-hydroxyvalerate)/poly(lactic acid)(PHBV/PLA)in blend fibers.After dissolving PHBV/PLA blend fibers in trichloromethane,characteristic methyl derivatives were obtained by the on-line derivatization in the presence of excess tetramethylammonium hydroxide(TMAH)under high temperature.Subsequently,the analysis of methyl derivatives was performed by the gas chromatographflame ionization detector-mass spectrometry.The calibration was linear in the range of 0.075-7.50μg for PHBV characteristic methylation product with a correlation coefficient(r)of 0.9954,while the calibration was linear in the range of 0.35-17.50μg for PLA characteristic methylation product with r of 0.9932.The limits of detection were 0.075μg and 0.35μg,the relative standard deviations(RSDs)were 6.0%and 4.8%,and the recoveries were 100.8%-107.6%and 91.3%-104.5%for PHBV and PLA characteristic methylation products,respectively.The proposed method demonstrated a significant potential in the application of identification and quantitative analysis of PHBV/PLA in blend fibers.

关 键 词：3-羟基丁酸-戊酸酯/聚乳酸 混合纤维 热辅助在线衍生化-气相色谱法 定量分析 

分 类 号：O657.31[理学—分析化学] X832[理学—化学]