目的采用LC/MSn技术推断拉氧头孢钠原料中杂质的结构。方法采用Shiseido TYPE UG80C18(4.6mm×250mm,5μm)色谱柱,以0.01mol/L醋酸铵溶液-甲醇(99:1,V/V)作为流动相A,以0.01mol/L醋酸铵溶液-甲醇(70:30,V/V)为流动相B,进行梯度洗脱...目的采用LC/MSn技术推断拉氧头孢钠原料中杂质的结构。方法采用Shiseido TYPE UG80C18(4.6mm×250mm,5μm)色谱柱,以0.01mol/L醋酸铵溶液-甲醇(99:1,V/V)作为流动相A,以0.01mol/L醋酸铵溶液-甲醇(70:30,V/V)为流动相B,进行梯度洗脱分离杂质。通过强力试验归属杂质的来源,在正离子模式下获取各杂质的质谱数据,结合头孢菌素的普遍质谱裂解规律和降解反应原理,解析相关杂质的结构。结果推断了12种杂质的化学结构,样品中未检出聚合物杂质。结论LC/MSn法可快速准确推断拉氧头孢钠原料中杂质结构,中国药典的拉氧头孢钠质量标准需要进一步提高。展开更多
The impurities in ethyl-2-[[2′-cyanobiphenyl-4-yl] methyl] amino]-3-nitrobenzoate,an intermediate for synthesis of candesartan cilexiti,were detected by LC-MSn. The structural assignment of these impurities was carri...The impurities in ethyl-2-[[2′-cyanobiphenyl-4-yl] methyl] amino]-3-nitrobenzoate,an intermediate for synthesis of candesartan cilexiti,were detected by LC-MSn. The structural assignment of these impurities was carried out by LC-MSn using electrospray ionization source and an ion trap mass analyzer. The formation of the impurities was discussed. Also the fragmentation pathways of these compounds were studied.展开更多
文摘目的采用LC/MSn技术推断拉氧头孢钠原料中杂质的结构。方法采用Shiseido TYPE UG80C18(4.6mm×250mm,5μm)色谱柱,以0.01mol/L醋酸铵溶液-甲醇(99:1,V/V)作为流动相A,以0.01mol/L醋酸铵溶液-甲醇(70:30,V/V)为流动相B,进行梯度洗脱分离杂质。通过强力试验归属杂质的来源,在正离子模式下获取各杂质的质谱数据,结合头孢菌素的普遍质谱裂解规律和降解反应原理,解析相关杂质的结构。结果推断了12种杂质的化学结构,样品中未检出聚合物杂质。结论LC/MSn法可快速准确推断拉氧头孢钠原料中杂质结构,中国药典的拉氧头孢钠质量标准需要进一步提高。
文摘The impurities in ethyl-2-[[2′-cyanobiphenyl-4-yl] methyl] amino]-3-nitrobenzoate,an intermediate for synthesis of candesartan cilexiti,were detected by LC-MSn. The structural assignment of these impurities was carried out by LC-MSn using electrospray ionization source and an ion trap mass analyzer. The formation of the impurities was discussed. Also the fragmentation pathways of these compounds were studied.
