qHNMR法测定5种苯磺酸酯类化合物的含量

Quantitative analysis of five benzenesulfonate ester compounds by qHNMR

摘要

目的: 建立qHNMR法测定苯磺酸甲酯、苯磺酸丙酯、苯磺酸异丙酯、对甲苯磺酸甲酯和对甲苯磺酸异丙酯等5种苯磺酸酯类化合物含量的方法。方法: 采用Bruker ANANCE NEO 600型核磁共振波谱仪采集一维核磁氢谱,30°脉冲,弛豫延迟时间(D1)10 s,扫描次数(NS)16次,测定温度25 ℃,分别以对苯二甲酸二甲酯为内标物,采用氘代氯仿(CDCl₃-d)为溶剂,对苯磺酸酯类化合物进行定量研究。结果: 采用对苯二甲酸二甲酯为内标物,通过qHNMR法测定5种苯磺酸酯类化合物的含量与质量平衡法所得结果基本一致。结论: 本研究建立的qHNMR法操作简单、快速、准确,可用于苯磺酸酯类化合物的含量测定,为此类标准物质准确赋值提供有力的佐证数据。

Abstract

Objective: To establish quantitative proton nuclear magnetic resonance (qHNMR) method to determine the contents of methyl benzenesulfonate, propyl benzenesulfonate, isopropyl benzenesulfonate, methyl p-toluenesulfonate, and isopropyl p-toluenesulfonate. Methods: Proton nuclear magnetic resonance spectroscopy (qHNMR) spectra were collected by BRUKEANANCE NEO 600 MHz NMR spectrometer. The parameters were set up as follows: 30° pulse sequences, the relaxation delay time was 10 s, the number for scanning was 16, and the experiment temperature was controlled at 25 ℃, dimethyl terephthalate were used as internal standard, respectively. The quantitative study of benzenesulfonate ester compounds was carried out in CDCl₃-d as solvents. Results: Using dimethyl terephthalate as internal standard, the contents of five benzenesulfonate ester compounds determined by qHNMR method were basically consistent with the results obtained by mass balance method. Conclusion: The qHNMR method established in this study is simple, rapid, and accurate, and can be used for the determination of benzenesulfonate ester compounds, providing strong evidence data for the accurate assignment of the reference material.

关键词

qHNMR法 / 苯磺酸酯类化合物 / 基因毒性 / 对苯二甲酸二甲酯

Key words

qHNMR / benzenesulfonate ester compounds / genotoxicity / dimethyl terephthalate