目的 考察N-亚硝基-N-甲基-4-氨基丁酸(NMBA)对照品的稳定性。方法 分别采用甲醇和乙腈作为溶剂,考察NMBA对照品溶液在4 ℃下24 h的稳定性以及25、40 ℃下1、3、7和10 d的短期稳定性,用高效液相色谱法(HPLC)测定纯度变化进行稳定性评估。利用高分辨质谱和核磁共振波谱对生成产物进行结构鉴定。结果 不同溶剂和不同温度变化对NMBA稳定性影响不同,在乙腈溶剂中比较稳定,在甲醇溶剂中4 ℃下24 h稳定,但其纯度在25、40 ℃均有不同程度的降低,尤其40 ℃放置10 d后,生成杂质约92%,经高分辨质谱和核磁共振波谱分析,生成产物为N-亚硝基-N-甲基-4-氨基丁酸甲酯。结论 通过对NMBA稳定性考察,为该对照品研制过程中溶剂的合理选择以及该对照品储存和用户的正确使用提供参考。
Abstract
OBJECTIVE To investigate the stability of N-nitroso-N-methyl-4-aminobutyric acid (NMBA) reference substance. METHODS Using methanol and acetonitrile as solvents, the stability of N-nitroso-N-methyl-4-aminobutyric acid (NMBA) reference substance at 4 ℃ for 24 h and short-term stability at 25 ℃ and 40 ℃ for 1, 3, 7 and 10 d were investigated, and the stability was evaluated by HPLC determination of purity. RESULTS Different solvents and temperature changes had different effects on the stability of NMBA. NMBA was relatively stable in acetonitrile. Although NMBA in methanol was stable at 4 ℃ for 24 h, it had different degrees of degradation at 25 ℃ and 40 ℃. Especially at 40 ℃ for 10 d, the degradation rate was about 92%. By high resolution mass spectrometry and NMR qualitative analysis, the degradation product was identified to be N-nitroso-N-methyl-4-aminobutyric acid methyl ester. CONCLUSION The stability of NMBA is investigated, which provides reference for the rational selection of solvent and the correct use of NMBA.
关键词
N-亚硝基-N-甲基-4-氨基丁酸 /
对照品 /
稳定性 /
结构鉴定
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Key words
NMBA /
reference standard /
stability /
structural identification
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中图分类号：
R917
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参考文献
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