基质辅助激光解吸电离飞行时间质谱法用于非极性聚合物的分析

引用本文: 李仕诚, 李明慧, 陈子龙, 朱新海. 基质辅助激光解吸电离飞行时间质谱法用于非极性聚合物的分析[J]. 分析化学, 2022, 50(1): 82-91. doi: 10.19756/j.issn.0253-3820.210593 shu

Citation: LI Shi-Cheng, LI Ming-Hui, CHEN Zi-Long, ZHU Xin-Hai. Analysis of Nonpolar Polymers by Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2022, 50(1): 82-91. doi: 10.19756/j.issn.0253-3820.210593 shu

基质辅助激光解吸电离飞行时间质谱法用于非极性聚合物的分析

李仕诚 ^1, ,
李明慧 ^2, ,
陈子龙 ^3, ,
朱新海 ^{3,
,}

1.
中山大学材料科学与工程学院, 广州 510006;
2.
中山大学化学学院, 广州 510006;
3.
中山大学测试中心, 广州 510275

通讯作者: 朱新海,E-mail:zhuxinh@mail.sysu.edu.cn

摘要: 对基质辅助激光解吸电离飞行时间质谱（MALDI-TOF MS）分析非极性聚合物时离子化试剂对测试结果的影响进行了研究。通过对比，选择反式-2-[3-（4-叔丁基苯基）-2-甲基-亚丙烯基]丙二腈（DCTB）为基质，以聚丁二烯（PB5000）、不同聚合度的聚苯乙烯（PS）、聚乙烯（PE2000）为样品，考察了9种铜盐的促离子化作用。结果表明，在相同的仪器测试条件下，Cu （NO₃）₂作为离子化试剂对3类非极性聚合物的分析均能获得具有最佳信号强度和分辨率的质谱图。以PB5000为分析对象，利用冷场扫描电子显微镜（SEM）进行分析，结果表明，相比于其它铜盐，Cu （NO₃）₂与PB5000、DCTB混合干燥后可得到更均匀的样品结晶。以DCTB为基质，Cu （NO₃）₂为阳离子化试剂，利用薄层色谱-基质辅助激光解吸电离飞行时间质谱（TLC-MALDI-TOF MS）联用技术，可以显著降低易于离子化的小分子盐（碘化钠）或其它聚合物（聚乙二醇）等杂质在MALDI-TOF MS分析时的离子抑制作用，实现了对杂质掺杂的聚合物PB5000和PS4000的有效分析。本方法速度快、成本低、操作简便，为低纯度非极性聚合物的MALDI-TOF MS分析提供了有效的解决方案。

关键词:

English

Analysis of Nonpolar Polymers by Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

1.
School of Materials Science and Engineering, Sun Yat-sen University, Guangzhou 510006, China;
2.
School of Chemistry, Sun Yat-sen University, Guangzhou 510006, China;
3.
Instrumental Analysis & Research Center, Sun Yat-sen University, Guangzhou 510275, China

Corresponding author: ZHU Xin-Hai, zhuxinh@mail.sysu.edu.cn

Received Date: 28 June 2021
Revised Date: 18 November 2021

Abstract: The influence of ionization reagent on the determination results of non-polar polymers by matrix assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) was investigated. As a comparison, trans-2-[3-(4-tert-butylphenyl)-2-methyl-propylene] malononitrile (DCTB) was selected as the matrix, and polybutadiene 5000 (PB5000), polystyrene (PS) with different degree of polymerization and polyethylene 2000 (PE2000) were selected as the samples.The ionization of nine copper salts was investigated. The results showed that, under the same test conditions, copper nitrate could be used as an ionization reagent for the analysis of three kinds of non-polar polymers with the best signal intensity and resolution of the polymer spectra.In the analysis of PB5000, further cold-field scanning electron microscopy (SEM) analysis showed that copper nitrate mixed with PB5000 and DCTB could obtain more uniform crystallization in comparison with other copper salts.Using DCTC as the matrix and copper nitrate as the cation reagent, thin layer chromatography-matrix-assisted laser desorption ionization time of flight mass spectrometry (TLC-MALDI-TOF MS) coupling technology couldeffectively reduce or eliminate the influence of ion inhibition caused by dopants such as small molecule salt (sodium iodide) and other polymers (polyethylene glycol) which were easy to ionize in the analysis of polyolefin by MALDI-TOF. The effective analysis of impurity doped polymers PB5000 and PS4000 was realized successfully. This method had many advantages such as fast analysis speed, low cost and simple operation. This study provided an effective solution for MALDI-TOF MS analysis of low purity nonpolar polymers.

Key words:

Nonpolar polymers
/ Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry
/ Ionization reagent
/ Copper salt
/ Thin-layer chromatography

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

基质辅助激光解吸电离飞行时间质谱法用于非极性聚合物的分析

通讯作者: 朱新海,E-mail:zhuxinh@mail.sysu.edu.cn

English

Analysis of Nonpolar Polymers by Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

Corresponding author: ZHU Xin-Hai, zhuxinh@mail.sysu.edu.cn

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

基质辅助激光解吸电离飞行时间质谱法用于非极性聚合物的分析

通讯作者: 朱新海,E-mail:zhuxinh@mail.sysu.edu.cn

English

Analysis of Nonpolar Polymers by Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

Corresponding author: ZHU Xin-Hai, zhuxinh@mail.sysu.edu.cn

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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