定量核磁共振氢谱法测定5种N-亚硝胺类化合物的含量  

Determination of five N-nitrosamine compounds by quantitative proton nuclear magnetic resonance

作　　者：张雅军[1] 陈忠兰 徐翊雯 孙会敏[1] 吴先富[1] 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)

机构地区：[1]中国食品药品检定研究院,北京102629

出　　处：《中国新药杂志》2022年第13期1326-1330,共5页Chinese Journal of New Drugs

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.

关 键 词：定量核磁共振氢谱法 N-亚硝胺类化合物 含量测定 

分 类 号：R917[医药卫生—药物分析学]