1-甲基-4-亚硝基哌嗪国家标准物质的研制及其核磁定量考察

Establishment of National Reference Standard of 1-Methyl-4-nitrosopiperazine and Its Nuclear Magnetic Quantitative Investigation

关键词:  国家标准物质  1-甲基-4-亚硝基哌嗪  质量平衡法

Key words:  national reference standard  1-methyl-4-nitrosopiperazine  mass balance method

摘要:

目的 以1-甲基-4-亚硝基哌嗪为例，介绍亚硝胺类化合物标准物质研制过程，并讨论采用核磁定量方法分析时需注意的问题。方法 采用气质联用、红外光谱和核磁共振法对该原料进行结构确证，定量考察方面进行HPLC纯度分析及水分测定；采用质量平衡法计算1-甲基-4-亚硝基哌嗪的含量，同时辅以定量核磁共振法验证本批原料的含量。结果 本批1-甲基-4-亚硝基哌嗪原料结构准确，在定量核磁考察中发现采用不同内标物对核磁定值结果影响较大。结论 由于1-甲基-4-亚硝基哌嗪本身具有碱性，使得其在核磁定量分析中采用酸性内标物测定易降低含量数值，因此提示对于该类样品在核磁定量过程中应选择适宜的内标物。

Abstract:

OBJECTIVE To introduce the developing procedure of reference standards of nitrosamines by taking 1-methyl-4-nitrosopiperazine(MNP) as example and discuss the problems needing attention when using nuclear magnetic resonance(NMR) quantitative method. METHODS The structure of the material was confirmed by mass spectrometry, infrared spectrum and nuclear magnetic methods. In terms of quantitative assessment, the purity of the material was analyzed by HPLC, and the water was investigated. The content of MNP was determined by mass balance method, the content of the material was verified by NMR quantitative method. RESULTS MNP was consistent with its structure. In the quantitative NMR investigation, it was found that the use of different internal standards had a great impact on the calibration results. CONCLUSION Since MNP is basic, it is easy to reduce the final determination result by using an acidic internal standard in NMR quantitative analysis. Therefore, it is suggested that an appropriate internal standard should be selected for this kind of sample in the process of NMR quantitative determination.