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~3H标记亮氨酸中~2H的丰度测定及标记部位的分析

Analysis of the abundance and labelled position of deuterium in ~H-leucine

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【作者】 戴腾昌; 张建华; 周文达; 夏宗勤;

【Author】 Dai Tengchang Zhang Jianhua Zhou Wenda Xia Zongqin (Shanghai Second Medical College)

【机构】 上海第二医学院; 上海第二医学院;

【摘要】 <正> 用催化通2H2(3H2)的方法对合双键的前身物进行加2H2(3H2)反应以制备相应的标记化合物,理论上应是严格定位的。但实际上标记原子在分子中的分布常较复杂,对氚的核磁共振分析(TNMR)已发表若干实例。本文介绍用气相色谱-质谱联用仪(GC-MS)测定2H-亮氨酸的质谱图,分析其中2H原子分布的结果。

【Abstract】 DL-(4,5-2H)-leucine was prepared by catalytic deuteration of its double-bond pre- cursor. Its trifluoroacetyl butanolic ester derivative was prepared and the deuterlum content was estimated by GC-MS. Analysis of the m/e = 182 fragment by Biemann’s method revealed that the 2H content varied from 0 to 6. The percentage of molecules containing no deuterium atom was 16.4, indicating that the abundance of labelled molecules (regardless of the number of deuterium atoms in each molecule) was 83.6%. Calculated from the intensity of the fragments m/e = 182, 153, 140 by Biemann’s method the abundances of labelled atoms at different C positions of the leucine molecule was: C1-0%; C2-2.9%; C3-22.5%; C4, C5, C6-54.2% (average).

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