莱克多巴胺标准物质中的有机杂质鉴定分析

引用本文: 段磐辉, 孟珂, 张宜文, 高慧, 马康. 莱克多巴胺标准物质中的有机杂质鉴定分析[J]. 分析化学, 2021, 49(4): 554-562. doi: 10.19756/j.issn.0253-3820.211031 shu

Citation: DUAN Pan-Hui, MENG Ke, ZHANG Yi-Wen, GAO Hui, MA Kang. Identification of Organic Impurities in Ractopamine Reference Material[J]. Chinese Journal of Analytical Chemistry, 2021, 49(4): 554-562. doi: 10.19756/j.issn.0253-3820.211031 shu

莱克多巴胺标准物质中的有机杂质鉴定分析

段磐辉 ^1,2, ,
孟珂 ^3, ,
张宜文 ^4, ,
高慧 ^5, ,
马康 ^{1,
,}

1.
中国计量科学研究院, 北京 100029;
2.
北京化工大学化学学院, 北京 100029;
3.
江苏省计量科学研究院, 南京 210007;
4.
北京市计量检测科学研究院, 北京 100029;
5.
岛津企业管理(中国)有限公司, 北京 100020

通讯作者: 马康,E-mail:makang@nim.ac.cn

基金项目:
国家重点研发计划项目（Nos.2018YFF0212800，2018YFF0212801）和基本科研业务费项目（No.21-AKY-1960）资助。

摘要: 纯度标准物质是量值溯源的源头，纯度值与有机杂质的定性和定量分析结果直接相关。莱克多巴胺（Ractopamine，RAC）是一种合成的β-肾上腺受体激动剂，是典型瘦肉精类物质之一。本研究采用高效液相色谱-四极杆-飞行时间质谱（HPLC-Q-TOF/MS）对莱克多巴胺标准物质候选物中的有机杂质进行定性分析，鉴定出4种主要有机杂质A（m/z 286.1802）、B（m/z 316.1907）、C（m/z 438.2275）和D（m/z 372.2533），4种杂质的碎片离子峰质量数的质量偏差范围为-0.6~0.6 mDa，相对质量偏差为-3.7×10^-6~2.1×10^-6。利用高分辨质谱数据，建立了莱克多巴胺和有机杂质的质谱碎片离子的裂解途径，推断出杂质A为莱克多巴胺脱水、加氢的副产物，B、C、D是与莱克多巴胺拥有相同分子骨架结构的类似物。使用HPLC-IT-TOF/MS对有机杂质质谱碎片进行对比验证，结果表明，两种不同类型高分辨质谱测定的莱克多巴胺及其杂质的质谱碎片推断的结构式一致性良好。本研究为有机杂质的定性分析的结果验证提供了新思路。

关键词:

English

Identification of Organic Impurities in Ractopamine Reference Material

DUAN Pan-Hui ^1,2, ,
MENG Ke ^3, ,
ZHANG Yi-Wen ^4, ,
GAO Hui ^5, ,
MA Kang ^{1,
,}

1.
National Institute of Metrology of China, Beijing 100029, China;
2.
College of Chemistry, Beijing University of Chemical Technology, Beijing 100029, China;
3.
Jiangsu Institute of Metrology, Nanjing 210007, China;
4.
Beijing Institute of Metrology, Beijing 100029, China;
5.
Shimadzu(China) Limited Co, Beijing 100020, China

Corresponding author: MA Kang, makang@nim.ac.cn

Received Date: 14 January 2021
Revised Date: 02 March 2021
Fund Project:
Supported by the National Key Research and Development Program of China(Nos.2018YFF0212800, 2018YFF0212801) and the Basic Scientific Research Expenses(No.21-AKY-1960).

Abstract: Ractopamine (RAC) is a synthetic β-adrenergic receptor agonist and one of the lean meat powder substances. The purity standard substance is the source of the traceability of the value. In this work, the organic impurities in RAC were analyzed by high performance liquid chromatography quadrupole-time of flight mass spectrometry (HPLC-Q-TOF/MS), including 4 main organic impurities A (m/z 286.1802), B (m/z 316.1907), C (m/z 438.2275) and D (m/z 372.2533). The range of impurity's fragment ion peak mass deviation (m/z) was (-0.6-0.6) mDa and the relative mass deviation was from -3.7×10^-6 to 2.1×10^-6. Using mass spectrometry data, the fragmentation pathway of ractopamine and the fragment ions of organic impurities was established. It was inferred that impurity A was a byproduct of the dehydration and hydrogenation of ractopamine, and B, C, D and ractopamine had the same molecular skeleton structure. In addition, high-performance liquid chromatography ion trap-time of flight mass spectrometry (HPLC-IT-TOF/MS) was used to compare and verify the mass spectra fragments of organic impurities. The results showed that the two different types of mass spectrometry were consistnet. This study provided a new way of verifying results for the accurate qualitative determination of organic impurities.

Key words:

Ractopamine
/ Quadrupole-time of flight mass spectrometry
/ Ion trap-time of flight mass spectrometry
/ Organic impurities

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

莱克多巴胺标准物质中的有机杂质鉴定分析

通讯作者: 马康,E-mail:makang@nim.ac.cn

English

Identification of Organic Impurities in Ractopamine Reference Material

Corresponding author: MA Kang, makang@nim.ac.cn

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

莱克多巴胺标准物质中的有机杂质鉴定分析

通讯作者: 马康,E-mail:makang@nim.ac.cn

English

Identification of Organic Impurities in Ractopamine Reference Material

Corresponding author: MA Kang, makang@nim.ac.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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