13C3-三聚氰酸、15N3-三聚氰胺的合成工艺研究

¹³C₃-三聚氰酸、¹⁵N₃-三聚氰胺的合成工艺研究

摘要: 研究了以稳定性同位素标记物¹³C-尿素和¹⁵N-氯化铵为原料制备质谱检测用内标物¹³C₃-三聚氰酸、¹⁵N₃-三聚氰胺的合成工艺；考察了温度、压力、溶剂等对产品收率的影响，优化了合成工艺，以良好收率合成了同位素内标试剂¹³C₃-三聚氰酸和¹⁵N₃-三聚氰胺。产品经高效液相色谱（HPLC）、质谱（MS）检测，化学纯度＞99%，同位素丰度＞98%。以上结果提示，所合成的¹³C₃-三聚氰酸和¹⁵N₃-三聚氰胺可作为同位素内标使用。

Abstract: The syntheses of two labeled internal standards ¹⁵N₃-melamine and ¹³C₃-cyanuric acid were studied. The influences of parameters such as temperature, pressure and solvent on the yield of products were investigated. ¹⁵N₃-melamine and ¹³C₃-cyanuric acid were prepared with the common substrates ¹⁵NH₄Cl and ¹³C-urea. Both products were shown by mass spectrometry to be target compounds. Their chemical purity were more than 99% based on HPLC analysis. The results showed that both products could be used as standards without further purification.