LC-MS/MS法测定苯磺酸氨氯地平胶囊中两种潜在基因毒性杂质的含量  

Content Determination of Two Potential Genotoxic Impurities in Amlodipine Besylate Capsule by LC-MS/MS

作　　者：孙朗 石明睿[2] 熊志立 SUN Lang;SHI Mingrui;XIONG Zhili(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;LIVZON(GROUP)Pharmaceutical Factory,Zhuhai 519045,China)

机构地区：[1]沈阳药科大学药学院,沈阳110016 [2]丽珠集团丽珠制药厂,珠海519045

出　　处：《医药导报》2022年第12期1846-1849,共4页Herald of Medicine

摘　　要：目的建立液相色谱-质谱联用(LC-MS/MS)测定苯磺酸氨氯地平胶囊中2个非磺酸酯类潜在基因毒性杂质含量的方法。方法使用液相色谱-三重四级杆质谱联用仪,色谱柱为Agilent poroshell 120 EC-C_(18),流动相A为5 mmol·L^(-1)乙酸铵的0.1%甲酸溶液,B为0.1%甲酸乙腈溶液,流速为0.5 mL·min^(-1),梯度洗脱;电喷雾离子源,扫描方式为正离子模式-多反应监测(MRM)。结果两种潜在基因毒性杂质A和B浓度分别在4.51~45.12 ng·mL^(-1)(r=0.990)和4.39~43.93 ng·mL^(-1)(r=1.000)内线性关系良好,平均回收率分别为102.3%和102.6%,RSD分别为1.5%和1.0%;使用该方法对国产和原研进口的苯磺酸氨氯地平胶囊进行测定,均未检出上述潜在基因毒性杂质。结论所建立的LC/MS分析方法可靠有效,可为苯磺酸氨氯地平胶囊的质量控制提供参考依据。Objective To establish a method that can determine two non-sulfonate esters'potential genotoxic impurities in amlodipine besylate capsule by LC-MS/MS.Methods A LC-triple quadrupole mass spectrometer with Agilent poroshell 120 EC-C_(18) column was used,the flow rate was 0.5 mL·min^(-1),with gradient elution while mobile phase A was 5 mmol·L^(-1) ammonium acetate solution added 0.1%formic acid and mobile phase B was acetonitrile added 0.1%formic acid.The source was ESI,scanned in MRM mode.Results The good linear ranges of two potential genotoxic impurities were 4.51-45.12 ng·mL^(-1)(r=0.990)and 4.39-43.93 ng·mL^(-1)(r=1.000).The average recoveries were 102.3%and 102.6%,respectively,the RSD was 1.5%and 1.0%respectively;The above potential genetic impurities were not detected in the domestic and reference amlodipine besylate capsules by this method.Conclusion The established LC-MS/MS method is effective and reliable,and can be used to evaluate the quality control of amlodipine besylate capsules.

关 键 词：苯磺酸氨氯地平胶囊 基因毒性杂质 液质联用色谱法 含量测定 

分 类 号：R917[医药卫生—药物分析学] R972.4[医药卫生—药学]