同位素稳定标记亚硝胺的合成与分析作为药物杂质质量控制的质谱标准

IF 0.9 4区医学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of labelled compounds & radiopharmaceuticals Pub Date : 2022-12-29 DOI:10.1002/jlcr.4010

Volker Derdau, Martin Sandvoss

{"title":"同位素稳定标记亚硝胺的合成与分析作为药物杂质质量控制的质谱标准","authors":"Volker Derdau, Martin Sandvoss","doi":"10.1002/jlcr.4010","DOIUrl":null,"url":null,"abstract":"We describe a simple and easy pathway to synthesize nitrosamine mass spectrometry standards in good to moderate yields. N-alkylation of Boc-protected primary or secondary amines using stable isotope labeled alkyl halides yielded the key intermediates that were deprotected, and then, the nitrosamine was formed with sodium nitrite and sodium hydrogensulfate. Special attention to safety, disposal of waste, and surface cleaning was carried throughout.","PeriodicalId":16288,"journal":{"name":"Journal of labelled compounds & radiopharmaceuticals","volume":"66 2","pages":"41-46"},"PeriodicalIF":0.9000,"publicationDate":"2022-12-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Synthesis and analysis of isotopically stable labeled nitrosamines as mass spectrometry standards for drug impurity quality control\",\"authors\":\"Volker Derdau, Martin Sandvoss\",\"doi\":\"10.1002/jlcr.4010\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"We describe a simple and easy pathway to synthesize nitrosamine mass spectrometry standards in good to moderate yields. N-alkylation of Boc-protected primary or secondary amines using stable isotope labeled alkyl halides yielded the key intermediates that were deprotected, and then, the nitrosamine was formed with sodium nitrite and sodium hydrogensulfate. Special attention to safety, disposal of waste, and surface cleaning was carried throughout.\",\"PeriodicalId\":16288,\"journal\":{\"name\":\"Journal of labelled compounds & radiopharmaceuticals\",\"volume\":\"66 2\",\"pages\":\"41-46\"},\"PeriodicalIF\":0.9000,\"publicationDate\":\"2022-12-29\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of labelled compounds & radiopharmaceuticals\",\"FirstCategoryId\":\"3\",\"ListUrlMain\":\"https://onlinelibrary.wiley.com/doi/10.1002/jlcr.4010\",\"RegionNum\":4,\"RegionCategory\":\"医学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"BIOCHEMICAL RESEARCH METHODS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of labelled compounds & radiopharmaceuticals","FirstCategoryId":"3","ListUrlMain":"https://onlinelibrary.wiley.com/doi/10.1002/jlcr.4010","RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}

引用次数: 0

摘要

我们描述了一种简单易行的合成亚硝胺质谱标准品的方法，收率好到中等。用稳定同位素标记的卤代烃对boc保护的伯胺或仲胺进行n -烷基化反应，得到脱保护的关键中间体，然后与亚硝酸钠和硫酸氢钠生成亚硝胺。对安全、废物处理和表面清洁的特别关注贯穿始终。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

查看原文本刊更多论文

Synthesis and analysis of isotopically stable labeled nitrosamines as mass spectrometry standards for drug impurity quality control

We describe a simple and easy pathway to synthesize nitrosamine mass spectrometry standards in good to moderate yields. N-alkylation of Boc-protected primary or secondary amines using stable isotope labeled alkyl halides yielded the key intermediates that were deprotected, and then, the nitrosamine was formed with sodium nitrite and sodium hydrogensulfate. Special attention to safety, disposal of waste, and surface cleaning was carried throughout.

求助全文

通过发布文献求助，成功后即可免费获取论文全文。去求助

来源期刊

Journal of labelled compounds & radiopharmaceuticals 医学-分析化学

CiteScore

3.30

自引率

0.00%

发文量

审稿时长

1 months

期刊介绍： The Journal of Labelled Compounds and Radiopharmaceuticals publishes all aspects of research dealing with labeled compound preparation and applications of these compounds. This includes tracer methods used in medical, pharmacological, biological, biochemical and chemical research in vitro and in vivo. The Journal of Labelled Compounds and Radiopharmaceuticals devotes particular attention to biomedical research, diagnostic and therapeutic applications of radiopharmaceuticals, covering all stages of development from basic metabolic research and technological development to preclinical and clinical studies based on physically and chemically well characterized molecular structures, coordination compounds and nano-particles.