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| Determination of Eight Kinds of Biogenic Amine Hydrochlorides by Nuclear Magnetic Resonance |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:biogenic amine hydrochloride biogenic amine quantitative nuclear magnetic resonance nuclear magnetic resonance purity assessment |
| Author | Institution |
| ZHANG Wei,HUANG Liang,XU Rui-feng,TU Guang-zhong,HUANG Ting,DAI Xin-hua,HE Ya-juan,LI Hong-mei |
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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| Abstract: |
| 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. |
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