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对安吡昔康(1)工艺中产生的杂质进行分离、提纯,采用LC-MS及1H NMR进行结构确证为6-甲基-6H-7-氧代吡啶并[1,2-a]嘧啶并[5,4-c]-1,2-苯并噻嗪-5,5-二氧化物(3)。建立了高效液相色谱法测定1的有关物质。采用ODS色谱柱,以0.05 mol/L磷酸二氢钾溶液(用磷酸调至pH 4.5)-乙腈为流动相,梯度洗脱,检测波长314 nm。1的有关物质吡罗昔康(2)和3在0.3～1 g/ml浓度范围内线性关系良好,平均回收率为105.0%和100.8%,RSD为1.19%和0.91%。
The impurities produced in the process of amiloxaban (1) were separated and purified, and the structures were confirmed by LC-MS and 1H NMR as 6-methyl-6H-7-oxopyrido [1,2-a] pyrimidine And [5,4-c] -1,2-benzothiazine-5,5-dioxide (3). The establishment of a high performance liquid chromatography determination of 1 related substances. ODS column was used with 0.05 mol / L potassium dihydrogen phosphate solution (adjusted to pH 4.5 with phosphoric acid) -acetonitrile as the mobile phase and gradient elution. The detection wavelength was 314 nm. The correlation between piroxicam (2) and 3 in the concentration range of 0.3-1 g / ml was good with the average recoveries of 105.0% and 100.8% with RSDs of 1.19% and 0.91%, respectively.