| 引用本文: | 王建,周萍,刘贵君,梁键谋,曹粤锋,张凤妹,邵鹏.HPLC-MS/MS分析阿哌沙班中基因毒性杂质及基质效应消除研究[J].中国现代应用药学,2022,39(10):1336-1341. |
| WANG Jian,ZHOU Ping,LIU Gui-jun,LIANG Jian-mou,CAO Yue-feng,ZHANG Feng-mei,SHAO Peng.Study on Genotoxic Impurities and Elimination of Matrix Effect in Apixaban by HPLC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2022,39(10):1336-1341. |
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| HPLC-MS/MS分析阿哌沙班中基因毒性杂质及基质效应消除研究 |
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王建1,2, 周萍1, 刘贵君1, 梁键谋2, 曹粤锋2, 张凤妹2, 邵鹏2,3
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1.浙江工业大学, 杭州 310014;2.浙江省食品药品检验研究院, 杭州 310052;3.浙江省原料药安全研究中心, 杭州 310051
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| 摘要: |
| 目的 建立HPLC-MS/MS测定阿哌沙班中基因毒性杂质胺化物、开链酰胺和肼基物的方法。方法 色谱柱为Zobax Eclipse XDB C18(3.0 mm×150 mm,3.5μm);胺化物和开链酰胺测定采用梯度洗脱法,流动相A为10 mmol·L-1乙酸铵溶液,流动相B为乙腈;肼基物测定采用等度法,流动相为水-甲醇(30∶70)。电喷雾离子化法在正离子模式下进行多重反应离子监测结构确认。结果 胺化物、开链酰胺和肼基物平均回收率分别为99.6%,92.2%和97.5%,RSD分别为3.8%,1.9%和7.2%(n=9);定量限分别为0.05,0.05,0.05 ng·mL-1。结论 该方法有效地消除了分析中出现的基质效应,可用于阿哌沙班中基因毒性杂质的定量检测。 |
| 关键词: 阿哌沙班 基因毒性杂质 基质效应 液相色谱-质谱联用法 |
| DOI：10.13748/j.cnki.issn1007-7693.2022.10.012 |
| 分类号:R973 |
| 基金项目:浙江省基础公益研究计划(LGC19H300002) |
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| Study on Genotoxic Impurities and Elimination of Matrix Effect in Apixaban by HPLC-MS/MS |
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WANG Jian1,2, ZHOU Ping1, LIU Gui-jun1, LIANG Jian-mou2, CAO Yue-feng2, ZHANG Feng-mei2, SHAO Peng2,3
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1.Zhejiang University of Technology, Hangzhou 310014, China;2.Zhejiang Institute for Food and Drug Control, Hangzhou 310052, China;3.Zhejiang Research Center for API Security, Hangzhou 310051, China
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| Abstract: |
| OBJECTIVE To establish an HPLC-MS/MS method for the determination of amines,open-chain amides and hydrazine based compound in apixaban.METHODS Separation was performed on a Zobax Eclipse XDB C18(3.0 mm×150 mm,3.5μm).Amines and open-chain amides were separated with the mobile phase of 10 mmol·L-1 ammonium acetate solution and acetonitrile in gradient elution.Hydrazine based compound was separated with the mobile phase of water-methanol(30:70) in isocratic elution.The electrospray ionization source with positive ion mode was used for structure confirmation in the multiple reaction monitoring(MRM) mode.RESULTS The average recoveries for the determination of amines,open-chain amides and hydrazine based compounds were 99.6%,92.2%and 97.5%,RSDs were 3.8%,1.9%and 7.2%(n=9),respectively.Limits of quantitation were 0.05,0.05 and 0.05 ng·mL-1.CONCLUSION The method can effectively eliminate the matrix effect and can be used for the quantitative determination of amines,open-chain amides and hydrazine based compound in apixaban. |
| Key words: apixaban genotoxic impurities matrix effect HPLC-MS/MS |
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