丹参酰-L-丙氨酰-L-脯氨酸冰片酯单晶的制备及其结构表征

目的 制备丹参酰-L-丙氨酰-L-脯氨酸冰片酯的单晶，并对其进行结构表征。方法 通过溶剂挥发法制备单晶，采用X射线单晶衍射对其晶体空间结构进行了解析，采用X射线粉末衍射进行晶型分析，通过热重分析（TGA）法–差示扫描量热法（DSC）分析热稳定性。结果 晶体呈现无色透明针状，属于单斜晶系，空间群为P2₁。1个晶胞由4个分子组成，氢键主要存在于分子间，分子中存在6个手性碳原子，R、S型各有3个碳原子。粉末X射线衍射实测粉末衍射图特征峰位置与理论衍射峰大致相同。DSC结果与TGA图结果一致。结论 确证了丹参酰-L-丙氨酰-L-脯氨酸冰片酯的立体构型和热稳定性。

Preparation and structure confirmation of tanshinol acyl-L-alanyl-L-proline bornyl ester single crystal

Objective To prepare single crystals of tanshinol acyl-L-alanyl-L-proline bornyl ester, and to characterize its structure. Methods Solvent evaporation method was used to grow single crystals. The spatial structure of the crystal was analyzed using X-ray single crystal diffraction, the crystal structure was analyzed using X-ray powder diffraction, and the thermal stability was analyzed using TGA-DSC. Results The crystal appeared colorless and transparent needle like, belonging to the monoclinic crystal system, with space group of P2₁. A crystal cell was composed of four molecules, with hydrogen bonds mainly presented between molecules. There were six chiral carbon atoms in the molecule, and three carbon atoms in each of the R and S types. The position of the characteristic peaks in the measured powder X-ray diffraction pattern was roughly the same as the theoretical diffraction peak. The DSC results were consistent with the TGA plot results. Conclusion Three-dimensional configuration and thermal stability of tanshinol acyl-L-alanyl-L-proline bornyl ester are confirmed.