LC-MS/MS法测定苹果酸舒尼替尼中潜在基因毒性杂质的含量  

LC-MS/MS determination of potential genotoxic impurities in sunitinib malate

作　　者：乔乔 彭厚霖 赵云丽[1] QIAO Qiao;PENG Houlin;ZHAO Yunli(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;Jiangsu Hansoh Pharmaceutical Group Co.,Ltd.,Lianyunsans 222000,China;No.9 Middle School of Shenyang,Shenyang 110015,China)

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016 [2]江苏豪森药业集团有限公司,江苏连云港222000 [3]沈阳市第九中学,辽宁沈阳110015

出　　处：《沈阳药科大学学报》2022年第4期387-392,共6页Journal of Shenyang Pharmaceutical University

摘　　要：目的建立LC-MS/MS法测定苹果酸舒尼替尼中3种潜在的基因毒性杂质的含量。方法采用Phenomenex Gemini C_(18)(100 mm×2.0 mm,3μm)色谱柱;流动相A为体积分数0.05%氨水,流动相B为乙腈,进行梯度洗脱。质谱采用电喷雾离子源(electron spray ionization,ESI),杂质A_(3)、B_(2)扫描模式为ESI(-),杂质A_(5)扫描模式为ESI(+)。结果杂质A_(3)、A_(5)和B_(2)在各自质量浓度范围内线性关系良好,定量限分别为0.5、1.0和0.5μg·L^(-1),检测限分别为0.1、0.5和0.1μg·L^(-1)。杂质A_(3)平均回收率为92.5%,RSD为4.0%;杂质A_(5)平均回收率为94.4%,RSD为5.1%;杂质B_(2)平均回收率为98.8%,RSD为6.5%。结论本方法可用于苹果酸舒尼替尼中潜在基因毒性杂质的检测。Objective To establish an LC-MS/MS analytical method for the determination of three potential genotoxic impurities in sunitinib malate.Methods A Phenomenex Gemini C_(18)(100 mm×2.0 mm,3μm)chromatographic column was used;mobile phase A was 0.05%ammonia and mobile phase B was acetonitrile with gradient elution.The electron spray ionization(ESI)was used for mass spectrometry,the scan mode of impurity A_(3) and B_(2) was ESI(-),and the scan mode of impurity A_(5) was ESI(+).Results The linear relationships of impurities A_(3),A_(5) and B_(2) were good in their respective ranges.The limits of quantitation were 0.5,1.0 and 0.5μg·L^(-1),and the limits of detection were 0.1,0.5 and 0.1μg·L^(-1),respectively.The average recovery rate of impurity A_(3) was 92.5%,and the RSD was 4.0%;the average recovery rate of impurity A_(5) was 94.4%,and the RSD was 5.1%;the average recovery rate of impurity B_(2) was 98.8%,and the RSD was 6.5%.Conclusion The method is simple and accurate,and can be used for the detection of potential genotoxic impurities in sunitinib malate.

关 键 词：苹果酸舒尼替尼 潜在基因毒性杂质 LC-MS/MS 

分 类 号：R917[医药卫生—药物分析学]