高分辨质谱测定氘标记化合物同位素分布与丰度的方法研究

引用本文: 田甜, 刘书妤, 李双青, 李秀琴, 张庆合. 高分辨质谱测定氘标记化合物同位素分布与丰度的方法研究[J]. 分析化学, 2021, 49(4): 563-570. doi: 10.19756/j.issn.0253-3820.201620 shu

Citation: TIAN Tian, LIU Shu-Yu, LI Shuang-Qing, LI Xiu-Qin, ZHANG Qing-He. Determination of Isotope Distribution and Abundance of Deuterium Labeled Compounds by High Resolution Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2021, 49(4): 563-570. doi: 10.19756/j.issn.0253-3820.201620 shu

高分辨质谱测定氘标记化合物同位素分布与丰度的方法研究

田甜 ^1,2, ,
刘书妤 ^{1,
,} ,
李双青 ^2, ,
李秀琴 ^{2,
,} ,
张庆合 ^2,

1.
上海工程技术大学, 上海 201620;
2.
中国计量科学研究院化学计量与分析科学研究所, 北京 100029

通讯作者: 刘书妤,E-mail:liushuyu1219@163.com; 李秀琴,E-mail:lixq@nim.ac.cn

基金项目:
中国计量科学研究院基本业务费项目（Nos.AKY1956，AKY1924）资助。

摘要: 采用四极杆轨道阱高分辨质谱，建立了快速检测氘标记化合物同位素分布与丰度的新方法。首先，建立仪器质量数偏差（IME）和同位素偏差（ID）的计算方法；其次，确定方法的适用前提为仪器质量偏差小于同位素偏差（即IME9（TMQ-D₉）模型物进行分析，考察测量允许偏差（Δ）和提取质谱图数量对同位素分布和丰度测量结果的影响。结果表明，在测量允许偏差（Δ）小于同位素偏差条件下，提取质谱图数量≥10张时，测量结果准确可靠。采用本方法测定TMQ-D₉和9种氘标记β-受体激动剂同位素分布与丰度，并将检测结果与"质量簇"分类和标准品标识同位素丰度值进行比较，结果表明，本方法灵敏度更高、同位素分布测量更准确。本方法快速简单，适于推广应用。

关键词:

English

Determination of Isotope Distribution and Abundance of Deuterium Labeled Compounds by High Resolution Mass Spectrometry

1.
College of Chemistry and Chemical Engineering, Shanghai University of Engineering Science, Shanghai 201620, China;
2.
Division of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, China

Corresponding author: LIU Shu-Yu, ; LI Xiu-Qin,

Received Date: 23 October 2020
Revised Date: 16 February 2021
Fund Project:
Supported by the Basic Research Project of National Institute of Metrology, China (Nos.AKY1956, AKY1924).

Abstract: A new method for rapid detection of isotope distribution and abundance of deuterium-labeled compounds by quadrupole orbitrap high resolution mass spectrometry (Q-Orbitrap HRMS) was devoloped. The calculation methods of instrument mass deviation (IME) and isotope deviation (ID) were established firstly. Then, the applicable conditions of the method were defined, that was, instrument mass deviation was less than the isotope deviation (IME9 (TMQ-D₉) as an example, a peristaltic pump was used to inject the analyte working solution (100 μg/kg), and the total ion current diagram (TIC) in 1 min was collected. Mass spectrums were selected every 0.1 min on the TIC, and a total of 10 typical spectra were obtained for analysis. The effects of the allowable deviation (Δ) and the analysis quantity of mass spectrometry on the isotopic distribution and abundance were investigated. The results showed that the measurement results were accurate and reliable when the (Δ) value was less than the ID value of the analyte and the analysis quantity of mass spectrum was more than 10 pieces. The method was applied to the analysis of isotope distribution and abundance of TMQ-D₉ and 9 deuterium-labeled β-receptor agonists, and the detection results were compared with the "Mass cluster" classification detection results and the isotope abundance values labeled on standard products. It was found that the established method had higher sensitivity, and could find more unlabeled compounds. Besides, it was more simple and rapid, and suitable for wide application.

Key words:

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沈阳化工大学材料科学与工程学院沈阳 110142

高分辨质谱测定氘标记化合物同位素分布与丰度的方法研究

通讯作者: 刘书妤,E-mail:liushuyu1219@163.com; 李秀琴,E-mail:lixq@nim.ac.cn

English

Determination of Isotope Distribution and Abundance of Deuterium Labeled Compounds by High Resolution Mass Spectrometry

Corresponding author: LIU Shu-Yu, ; LI Xiu-Qin,

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

高分辨质谱测定氘标记化合物同位素分布与丰度的方法研究

通讯作者: 刘书妤,E-mail:liushuyu1219@163.com; 李秀琴,E-mail:lixq@nim.ac.cn

English

Determination of Isotope Distribution and Abundance of Deuterium Labeled Compounds by High Resolution Mass Spectrometry

Corresponding author: LIU Shu-Yu, ; LI Xiu-Qin,

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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