气相色谱-质谱法检测纸张中的烷基烯酮二聚体施胶剂  

Determination of Alkyl Ketene Dimer Sizing Agent in Paper by Gas Chromatography-Mass Spectrometry

作　　者：张艺丹 杨瑞琴[1] 廉哲 ZHANG Yi-dan;YANG Rui-qin;LIAN Zhe(School of Criminal Investigation,People's Public Security University of China,Beijing 100038,China;Institute of Forensic Sciences,Ministry of Public Security,Beijing 100038,China)

机构地区：[1]中国人民公安大学侦查学院,北京100038 [2]公安部鉴定中心,北京100038

出　　处：《分析测试学报》2024年第3期464-473,共10页Journal of Instrumental Analysis

基　　金：中央级公益性科研院所基本科研业务费(2021JB014);公安理论及软科学研究计划(2016LLYJGAES017);中国人民公安大学刑事科学技术双一流创新研究专项(2023SYL06)。

摘　　要：建立了纸张中烷基烯酮二聚体施胶剂的水解提取结合气相色谱-质谱检测方法。纸张样品以1 mol/L氢氧化钠溶液在70℃恒温水浴条件下水解2 h后,以二氯甲烷静置萃取1 h,提取液经过滤后,待测物采用气相色谱-质谱法测定,以保留时间和特征离子对定性,内标法定量。结果表明:14-二十七酮、16-三十一酮和18-三十五烷酮分别在1.0~50 mg/L、1.0~50 mg/L和2.5~50 mg/L范围内线性关系良好,相关系数(r^(2))均大于0.98,检出限分别为0.1、0.5、2.0 mg/L,定量下限分别为0.5、1.5、5.0 mg/L。施胶量为1%的杨木纤维手抄纸样品中,基于平均留着率计算得到烷基烯酮二聚体的提取回收率为34.9%~60.9%。利用该方法测定40种不同品牌的静电复印纸,依据特征物质、烷基烯酮二聚体施胶剂原料配比和纸张中总酮含量将40种纸样分为三大类。该方法更简便、温和,适用于法庭科学领域纸张物证的检验与比对区分,可为纸张施胶方式研判、厂家溯源与形成年代推断提供新的参考依据。A hydrolytic extraction method combined with gas chromatography-mass spectrometry(GC-MS)method for the determination of alkyl ketene dimer sizing agent in paper was developed.The paper samples were hydrolyzed with 1 mol/L sodium hydroxide solution in a constant temperature water bath at 70℃for^(2) h,and then extracted with methylene chloride for 1 h.After the filtration of the extraction solution,the analytes were measured on GC-MS,characterized by retention time and characteristic ion pairs,and quantified by internal standard method.The results showed that there were good linear relations for the 14-heptacosanone,16-hentriacontanone and 18-pentatriacontanone in the range of 1.0-50 mg/L,1.0-50 mg/L,and 2.5-50 mg/L,respectively,with correlation coef⁃ficients(r^(2))more than 0.98.The limits of detection for the analytes were 0.1 mg/L,0.5 mg/L and 2.0 mg/L,and the limits of quantitation were 0.5 mg/L,1.5 mg/L and 5.0 mg/L,respectively.Based on the average retention,the extraction recovery of alkyl ketene dimer from poplar fiber handmade paper with sizing content of 1%were 34.9%-60.9%.The method was used to detect 40 kinds of different brands of copy paper.According to the characteristic substances,the ratio of raw materials for alkyl ketene dimer,and total ketone content in paper,40 kinds of paper samples were divided in⁃to three categories.The method is simpler and milder than existed ones,which is suitable for the ex⁃amination and comparison of paper material evidence in the field of forensic science.Besides,this method can provide a new reference for the research and judgment of paper sizing method,manufac⁃turer tracing,and formation age inference.

关 键 词：烷基烯酮二聚体 施胶剂 气相色谱-质谱法 纸张检验 法庭科学 

分 类 号：O657.63[理学—分析化学] DF794.3[理学—化学]