College of Chemical Engineering, Xiangtan University, Xiangtan, 411105, China.
Anal Bioanal Chem. 2024 Dec;416(29):6839-6847. doi: 10.1007/s00216-024-05580-7. Epub 2024 Oct 14.
In recent years, the control of volatile N-nitrosamines (NAs) has been of interest in the pharmaceutical and food industries, as many of these compounds are probable human carcinogens. Thus, rapid and trace-level quantitative determination methods are in urgent demand. In this work, ambient pressure ammonium-adduct ionization mass spectrometry was proposed for the sensitive detection of volatile nitrosamines in various pharmaceutical headspaces. The ammonium ions produced through electrospray ionization acted as reactant ions for NAs to generate ammonium-NA adduct ions and underwent in-source collision-induced dissociation to produce protonated NAs, which were detected by mass spectrometry. The ionization selectivity and sensitivity for various volatile NAs were improved significantly using the developed method, which was demonstrated by the limit of quantification (LOQ) below 52 ng L for all NAs, and the quantitative performance was consequently improved. Different NAs exhibited almost equimolar response using NH as the reactant ion, with at least a twofold enhancement in intensity for the individual compounds relative to when using H as the reactant ion. The proposed method is a rapid, sensitive, and environmentally economical approach that uses few reagents.
近年来，制药和食品行业一直关注挥发性 N-亚硝胺（NAs）的控制，因为许多此类化合物可能是人类致癌物。因此，迫切需要快速和痕量定量测定方法。在这项工作中，提出了环境压力铵加成电离质谱法，用于灵敏检测各种药物顶空的挥发性亚硝胺。通过电喷雾电离产生的铵离子作为 NAs 的反应离子，生成铵-NA 加合物离子，并在源内发生碰撞诱导解离，生成质子化的 NAs，通过质谱进行检测。开发的方法显著提高了各种挥发性 NAs 的电离选择性和灵敏度，所有 NAs 的定量下限（LOQ）均低于 52ng/L，因此定量性能得到了提高。使用 NH 作为反应离子时，不同的 NAs 表现出几乎等摩尔的响应，与使用 H 作为反应离子时相比，各化合物的强度至少增强了两倍。该方法快速、灵敏且环保，试剂用量少。
