摘要
目的:建立了测定N-亚硝基二正丙胺(N-nitrosodipropylamine,NDPA)、N-亚硝基二正丁胺(N-nitrosodibutylamine,NDBA)、N-亚硝基二异丙胺(N-nitrosodiisopropylamine,NDIPA)、N-亚硝基-N-甲基苯胺(N-nitroso-N-methylphenylamine,NMPA)和N-亚硝基-N-乙基苯胺(N-nitroso-N-ethylphenylamine,NEPA)5种N-亚硝胺类化合物含量的定量核磁共振氢谱法(quantitative proton nuclear magnetic resonance,qHNMR)。方法:采用BRUKER ANANCE NEO 600型核磁共振波谱仪采集一维核磁共振定量氢谱,以1,3,5-三甲氧基苯为内标,氘代二甲基亚砜(DMSO-d6)为溶剂,90°脉冲,采样次数为32次,采样时间为2.75 s,弛豫延迟时间(D1)为30 s,对5种N-亚硝胺类化合物进行定量研究。结果:5种N-亚硝胺类化合物qHNMR法的结果与质量平衡法结果基本一致。结论:本文建立的qHNMR法简单快捷,准确性高,为N-亚硝胺类化合物含量测定提供了新的方法,同时作为该类化学对照品质量平衡法定值结果的有力佐证,使质量平衡法赋值更加准确可靠。
Objective:To establish the quantitative proton nuclear magnetic resonance(qHNMR)method for N-nitrosodipropylamine(NDPA),N-nitrosodibutylamine(NDBA),N-nitrosodiisopropylamine(NDIPA),Nnitroso-N-methylphenylamine(NMPA)and N-nitroso-N-ethylphenylamine(NEPA).Methods:Proton nuclear magnetic resonance spectroscopy(~1 H NMR)spectra were collected by BRUKEANANCE NEO 600 MHz NMR spectrometer.1,3,5-Trimethoxybenzene was used as the internal standard and DMSO-d6 as solvent for the quantification of five N-nitrosamine compounds.The parameters were set up as follows:pulse sequence 90°,number for sampling was 32,acquisition time was 2.75 s,and relaxation delay time(D1)was 30 s.Results:The results of qHNMR of five N-nitrosamine compounds were basically consistent with those of mass balance method.Conclusion;The qHNMR method established in this paper is simple,rapid and accurate,providing a new detection method for the calibration of N-nitrosamine compounds.It can be used as the supporting evidence for the results of mass balance method,making the assignment of mass balance method more accurate and reliable.
作者
张雅军
陈忠兰
徐翊雯
孙会敏
吴先富
ZHANG Ya-jun;CHEN Zhong-lan;XU Yi-wen;SUN Hui-min;WU Xian-fu(National Institutes for Food and Drug Control,Beijing 102629,China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2022年第13期1326-1330,共5页
Chinese Journal of New Drugs
关键词
定量核磁共振氢谱法
N-亚硝胺类化合物
含量测定
quantitative proton nuclear magnetic resonance
N-nitrosamine compounds
content determination
