UPLC-MS法测定注射用盐酸表柔比星丁基橡胶塞中3个酰胺化合物的迁移量  

Determination of the Migration Quantity of Three Amides in Butyl Rubber Stopper for Injection of Epirubicin Hydrochloride by UPLC-MS

作　　者：郝贵周 陈晓杰 孙建合 侯继鹏 冯中 张贵民 HAO Guizhou;CHEN Xiaojie;SUN Jianhe;HOU Jipeng;FENG Zhong;ZHANG Guimin(National Engineering Research Center of Chiral Drugs,Lunan Pharmaceutical Group Co.,Lid.,Linyi 273400)

机构地区：[1]鲁南制药集团股份有限公司,国家手性制药工程技术研究中心,山东临沂273400

出　　处：《中国医药工业杂志》2022年第7期1034-1037,共4页Chinese Journal of Pharmaceuticals

摘　　要：建立了超高效液相色谱-质谱(UPLC-MS)法测定注射用盐酸表柔比星丁基橡胶塞中十六碳酰胺(2)、油酸酰胺(3)和硬脂酰胺(4)的迁移量。色谱柱采用Thermo Hypersil GOLD柱(2.1 mm×100 mm,3 μm),以0.1%甲酸溶液∶甲醇(15∶85)为流动相,等度洗脱。采用电喷雾离子源(ESI),正离子模式采集,单离子检测模式(SIM)。结果显示,2、3、4分别在0.039 2~0.783 6 μg/ml、0.040 0~0.800 2 μg/ml、0.037 3~0.746 0 μg/ml内线性关系良好。检测限分别为0.011 8、0.012 0、0.011 2 μg/ml;平均回收率(n=12)分别为96.28%、97.21%和94.11%,RSD分别为3.39%、4.22%和5.63%。建立的方法灵敏度高,专属性好,为注射用表柔比星的质量控制和安全性评价提供了参考。An ultra-high performance liquid chromatography-mass spectrometry(UPLC-MS) method was established for the determination of migration quantity of hexadecanamide(2),oleamide(3) and stearamide(4) from butyl rubber stopper for injection of epirubicin hydrochloride.The Thermo Hypersil GOLD column(2.1 mm×100 mm,3 μm) was used,and the analysis was carried out in the isocratic elution mode with 0.1% formic acid solution∶methanol(15∶85) as the mobile phase.Electrospray ionization(ESI),positive ion mode acquisition and single ion detection mode (SIM) were used.The results showed that it was linear for 2,3 and 4 in the ranges of 0.039 2-0.783 6 μg/ml,0.040 0-0.800 2 μg/ml and 0.037 3-0.746 0 μg/ml,respectively.The detection limits of 2,3 and 4 were 0.011 8,0.012 0,and 0.011 2 μg/ml,respectively,the mean recoveries(n=12) were 96.28%,97.21%,and 94.11%,with the RSDs of 3.39%,4.22%,and 5.63%,respectively.The established method has high sensitivity and good specificity,which provides a reference for the quality control and safety evaluation of epirubicin hydrochloride for injection.

关 键 词：注射用盐酸表柔比星 丁基橡胶塞 十六碳酰胺 油酸酰胺 硬脂酰胺 超高效液相色谱-质谱 

分 类 号：R917[医药卫生—药物分析学]