同时测定泮托拉唑钠中三种基因毒性杂质

Study on the Detection Method of genotoxicity Impurities in pantoprazole Sodium

关键词:  泮托拉唑钠  基因毒性杂质

Key words:  pantoprazole sodium  genotoxic impuriti

摘要:

目的 用同一个色谱-质谱条件检测泮托拉唑钠的三个基因毒性杂质。方法 采用色谱-质谱法,色谱条件：色谱柱为十八烷基硅烷键合硅胶为填充剂(Kromasil 100-5,4.6mm×25cm,5μm或效能相当的色谱柱),以乙腈-0.01 mol/L乙酸铵(35:65)为流动相,体积流速0.9ml/min,柱温25℃；质谱条件：正离子检测模式,扫描范围：150-450DA,干燥器温度350℃,干燥气流速10L/min,雾化气压力50psig,毛细管电压4000V,碎裂电压175V,锥孔电压65V。切入质谱的时间设为0~3.5min to waste,3.5~主峰保留时间-0.5min to MS,主峰保留时间-0.5min~end to waste。结果 该方法专属性、线性范围、检测限定量限、准确度、重复性、溶液稳定性均良好。结论 所建立的方法可用于泮托拉唑钠原料基因毒性杂质1、基因毒性杂质2、中间体Ⅱ三种基因毒性杂质的检测。

Abstract:

ABSTRACT: OBJECTIVE Detection of three genotoxicity impurities in pantoprazole sodium by the same chromatography-mass spectrometry condition. METHODS Using chromatography-mass spectrometry, chromatographic conditions: the chromatographic column is octadecylsilane bonded silica gel as the filling agent (Kromasil 100-5, 4.6mm × 25cm，5 μ M or equivalent chromatographic column, using acetonitrile -0.01 mol/L ammonium acetate (35:65) as the mobile phase, with a volumetric flow rate of 0.9 ml/min and a column temperature of 25 ℃; Mass spectrometry conditions: positive ion detection mode, scanning range: 150-450DA, dryer temperature 350 ℃, dry gas flow rate 10L/min, atomization gas pressure 50psig, capillary voltage 4000V, fragmentation voltage 175V, and cone hole voltage 65V. The time for entering the mass spectrometry is set to 0-3.5 minutes to waste, 3.5 minutes to retain the main peak -0.5 minutes to MS, and 0.5 minutes to end to waste. RESULTS The method has good specificity, linearity and range, detection limit and quantification limit, accuracy, repeatability, and solution stability.CONCLUSION The established method can be used for the detection of genotoxicity impurities 1, genotoxicity impurities 2 and intermediate II of pantoprazole sodium raw material genotoxicity impurities. KEY WORDS: pantoprazole sodium; genotoxic impurities