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蒿甲醚是菊科植物黄花蒿中分离的青蒿素还原并甲基化的β型产物,反应过程中有不少付产物,本文先用定量薄层层析法将产品中的杂质进行分离,然后用双波长薄层扫描仪将层析斑点进行测定,并根据工作曲线计算其含量。 1.仪器、试剂: (1)对二甲氨基苯甲醛试液:取对二甲氨基苯甲醛0.25g溶于50ml冰醋酸中和85％磷酸5g于20ml水中混合而成。 (2)岛津CS-910双波长薄层扫描仪。 2.展开剂的选择:以下二种溶剂系统均能得到满意的结果:(1)石油醚:醋酸乙酯=7∶3,蒿甲醚的R_f0.6,(2)苯:醋酸乙酯=9:1,蒿甲醚的R_f0.8。 3.显色剂的选择:经对1％硫酸香兰素,碘蒸汽,对二甲氨基苯甲醛等显色剂的实验。结果表明,以对二甲氨基苯甲醛试液为最佳。显色灵敏度为0.1γ,放置24小时稳定。
Artemether is artemisinin isolated from Artemisia annua artemisinin reduction and methylation of β-type products, the reaction process has many products to pay, this paper first quantitative thin-layer chromatography of impurities in the product were isolated , And then double-wavelength TLC scanner tomographic spots were measured and calculated according to the working curve of its content. 1. Instruments, reagents: (1) p-dimethylaminobenzaldehyde test solution: p-dimethylaminobenzaldehyde 0.25g dissolved in 50ml glacial acetic acid and 85% phosphoric acid 5g mixed in 20ml of water. (2) Shimadzu CS-910 dual-wavelength thin-layer scanner. 2.Expansion agent selection: The following two solvent systems can be satisfied with the results: (1) petroleum ether: ethyl acetate = 7: 3, artemether R_f0.6, (2) benzene: ethyl acetate = 9: 1, artemether R_f0.8. 3. The choice of developer: After 1% sulfuric acid vanillin, iodine vapor, p-dimethylaminobenzaldehyde and other developers experiment. The results show that p-dimethylaminobenzaldehyde test solution is the best. Color sensitivity of 0.1γ, placed 24 hours stable.