液相色谱-质谱联用鉴定抗菌肽Cbf-14凝胶的有关物质  

Identification of the related substances of antimicrobial peptide Cbf-14 gel by LC-MS

作　　者：霍怡彤 徐柯卉 陆宇婷 马菱蔓 周长林[2] 杭太俊[1] 宋敏[1] HUO Yitong;XU Kehui;LU Yuting;MA Lingman;ZHOU Changlin;HANG Taijun;SONG Min(School of Pharmacy,China Pharmaceutical University,Nanjing 211198;School of Life Science&Technology,China Pharmaceutical University,Nanjing 211198,China)

机构地区：[1]中国药科大学药学院,南京211198 [2]中国药科大学生命科学与技术学院,南京211198

出　　处：《中国药科大学学报》2022年第5期591-598,共8页Journal of China Pharmaceutical University

摘　　要：多肽Cbf-14是由14个氨基酸组成的新型抗菌肽。采用优化的反相高效液相色谱-电喷雾正离子化-四极杆飞行时间串联质谱(LC-ESI-QTOF/MS)检测方法,Agilent ZORBAX SB-Phenyl(150 mm×4.6 mm,3.5μm)色谱柱,以乙腈-20 mmol/L甲酸铵水溶液(甲酸调节pH为3.0)为流动相进行梯度洗脱,对Cbf-14凝胶中的有关物质进行了分离鉴定。在所建立的分析条件下,Cbf-14及其有关物质分离良好,检测并鉴定出Cbf-14凝胶及其强制降解试验样品中24个主要有关物质,其中5个为制剂生产工艺杂质,19个为降解产物,分析了有关物质的来源和多肽制剂的稳定性,为其生产工艺优化、贮存条件制定和质量控制提供了参考依据。Cbf-14 is a novel antimicrobial peptide composed of 14 amino acids.An optimized reversed phase high-performance liquid chromatographic method with electrospray-ionization quadrupole time-of-flight mass spectrometer(LC-ESI-QTOF/MS)method was developed for separation,identification and characterization of structurally related peptide impurities in Cbf-14 gel.Chromatographic separation was carried out on an Agilent ZORBAX SB-Phenyl column(150 mm×4.6 mm,3.5μm),with acetonitrile-20 mmol/L ammonium formate buffer(adjusted to pH 3.0 with formic acid)as eluent using gradient elution.Under the established conditions,Cbf-14 and its structurally related peptide impurities were well separated;and a total of 24 impurities were detected and identified,of which 5 were impurities in the preparation manufacturing process and 19 were stressed products.Based on high resolution mass spectrometry analysis,the origins and formation mechanisms of these impurities were located.The obtained results are useful for the establishment of the manufacturing process,storage condition and quality control of Cbf-14 gel.

关 键 词：抗菌肽Cbf-14凝胶 有关物质 结构鉴定 液相色谱-质谱联用 

分 类 号：R917[医药卫生—药物分析学]