1. 中国计量科学研究院化学计量与分析科学研究所
2. 广州计量检测技术研究院
3. 北京微量化学研究所
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张伟, 黄亮, 徐瑞峰, 等. 8种生物胺盐核磁共振法纯度定值[J]. 分析测试学报, 2014,33(8):940-945.
Determination of Eight Kinds of Biogenic Amine Hydrochlorides by Nuclear Magnetic Resonance[J]. 2014,33(8):940-945.
建立了核磁共振氢谱法(1H NMR)测定盐酸精胺、盐酸亚精胺、盐酸组胺、盐酸腐胺、盐酸尸胺、盐酸2-苯乙胺、盐酸酪胺和盐酸章胺8种生物胺盐酸盐纯度的定值方法。8种生物胺盐酸盐采用1H,1H-1H COSY谱对氢进行了归属,选择国家二级标准物质尼泊金乙酯(GBW(E)100064)为内标对8种生物胺盐酸盐进行纯度测定,并考察了不同实验参数对准确定量的影响,以标准物质尼泊金乙酯和对硝基甲苯对实验参数进行考察。实验结果显示,弛豫时间是影响定量的主要因素,准确定量时应采用远大于5倍T1(90度脉冲宽度)的弛豫时间,而脉冲宽度对定量结果无影响,但小的脉冲宽度可在确保定量准确性的前提下缩短弛豫时间。采用优化后的实验参数条件对8种生物胺盐酸盐进行定值,其纯度分别为99.0%,99.1%,99.4%,99.1%,99.3%,99.6%,99.6%,93.3%,相对标准偏差分别为0.2%,0.2%,0.3%,0.2%,0.2%,0.1%,0.2%,0.3%。
A method of nuclear magnetic resonance(qNMR) was established for the simultaneous determination of eight kinds of biogenic amine hydrochlorides(e.g.spermine tetrahydrochloride,spermidine trihydrochloride,histamine dihydrochloride,putrescine dihydrochloride,cadaverine dihydrochloride,2-phenylethylamine hydrochloride,tyramine hydrochloride and D1-octopamine hydrochloride).The hydrogen of eight kinds of biogenic amine hydrochlorides were assigned by 1H and 1H-1H COSY spectra,and the ethyl paraben(certified reference material,GBW(E)100064 ) was selected as the internal standard for the purity detection of biogenic amine hydrochlorides.The experimental parameters of NMR were extensively investigated to achieve optimal conditions.It was found that relaxation delay was the main factor affecting the accuracy of the quantitative analysis of qNMR.Two certified reference materials(CRM),ethyl paraben and p nitrotoluene,were chosen for the experiments of parameter selection.The experimental results indicated the five times of T1 was not sufficient for the accuracy of quantitative analysis of qNMR.The change of pulse width would not influence the experimental results of qNMR,but the use of narrow pulse width could reduce the time of relaxation delay.The eight kinds of biogenic amine hydrochlorides were detected by qNMR,and the purities for them were 99.0%,99.1%,99.4%,99.1%,99.3%,99.6%,99.6%,93.3%,with relative standard deviations(RSD) of 0.2%,0.2%,0.3%,0.2%,0.2%,0.1%,0.2%,0.3%,respectively.
生物胺盐酸盐生物胺定量核磁共振法核磁共振法纯度定值
biogenic amine hydrochloridebiogenic aminequantitative nuclear magnetic resonancenuclear magnetic resonancepurity assessment
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