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高效液相色谱-四极杆/线性离子阱质谱法同时测定艾司奥美拉唑钠中2种潜在基因毒性杂质残留
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作者单位
李锐,徐金梅,孙卫东,邬向东 河南中帅医药科技股份有限公司 
基金项目:河南省中国科学院科技成果转化转移项目(2012105)
中文摘要:建立了高效液相色谱-四极杆/线性离子阱质谱法(HPLC-QTRAP-MS/MS)同时测定艾司奥美拉唑钠中氮氧物(GTI E)和氮氧磺酰物(GTI I) 2种潜在基因毒性杂质痕量残留的分析方法。艾司奥美拉唑钠药物以30%(体积分数)乙腈水溶液溶解后,采用Agela VenusiL MP-C18色谱柱(2.1 mm×100 mm,3 μm)分离,以乙腈-水为流动相梯度洗脱,在流速0.2 mL/min,柱温35 ℃,进样量1 μL,电喷雾负离子(ESI-)扫描方式下以多反应离子监测(MRM)模式进行检测。结果表明,艾司奥美拉唑钠潜在基因毒性杂质GTI E和GTI I分别在1.26~44.8、1.34~45.2 μg/L范围内线性关系良好,相关系数(r)分别为0.994 7和0.992 8,检出限(S/N=3)分别为0.381、0.384 μg/L,定量下限分别为1.26、1.34 μg/L,平均加标回收率分别为86.3%~87.6%和85.8%~91.4%,相对标准偏差(RSDs)分别为1.5%~2.2%和0.7%~4.0%。该方法操作简单、灵敏度高、重现性好,可用于艾司奥美拉唑钠药物中GTI E和GTI I 2种潜在基因毒性杂质的同时测定。
中文关键词:高效液相色谱-四极杆线性离子阱质谱仪  艾司奥美拉唑钠  潜在基因毒性杂质
 
Simultaneous Determination of Two Potential Genotoxic Impurities Residues in Esomeprazole Sodium by HPLC-QTRAP-MS/MS
Abstract:A high performance liquid chromatography-quadrupole ion trap mass spectrometric(HPLC-QTRAP-MS/MS)method was developed for the determination of two potential genotoxic impurities residues,ieomeprazole N-oxide(GTI E)and sulfonylate N-oxide(GTI I)in esomeprazole sodium.The esomeprazole sodium drugs were dissolved with 30% acetonitrile-water(volume fraction),and then separated on an Agela VenusiL MP-C18 column(21 mm×100 mm,3 μm)by gradient elution using water-acetonitrile as mobile phases at a flow rate of 0.2 mL/min,a column temperature of 35 ℃ and an injection volume of 1 μL.The detection of analytes was performed in the negative electrospray ionization mode(ESI-)under multiple reaction monitoring(MRM)mode.As a result,the calibration curves for GTI E and GTI I showed good linearities in the ranges of 1.26-44.8 μg/L and 1.34-45.2 μg/L,with their correlation coefficients of 0.994 7 and 0.992 8,respectively.The limits of detection(S/N=3)and limits of quantitation(S/N=10)of the method were 0.381 and 0.384 μg/L,and 1.26 and 1.34 μg/L,respectively.The spiked recoveries for GTI E and GTI I were in the ranges of 86.3%-87.6% and 85.8%-91.4%,with the relative standard deviations(RSDs)of 1.5%-2.2% and 0.7%-4.0%,respectively.The method has the advantages of simple operation,high sensitivity,good reproducibility,and could be used for the simultaneous detection of two potential genotoxic impurities including GTI E and GTI I in esomeprazole sodium.
Key Words:high performance liquid chromatography-quadrupole ion trap mass spectrometry(HPLC-QTRAP-MS/MS)  esomeprazole sodium  potential genotoxic impurities
引用本文:李锐,徐金梅,孙卫东,邬向东.高效液相色谱-四极杆/线性离子阱质谱法同时测定艾司奥美拉唑钠中2种潜在基因毒性杂质残留[J].分析测试学报,2019,(4):449-454.
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