2D-LC-IT-TOF-MS/MS联用Cef-SEC法测定注射用盐酸头孢吡肟中的多聚体杂质  

Determination of the Polymer Impurities in Cefepime Hydrochloride for Injection by Cef-SEC Combined with 2D-LC-IT-TOF-MS/MS

作　　者：韩彬 王强 杨天风 田兰 高燕霞 Han Bin;Wang Qiang;Yang Tianfeng;Tian Lan;Gao Yanxia(Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050011,China)

机构地区：[1]河北省药品医疗器械检验研究院,石家庄050051

出　　处：《中国药师》2022年第3期449-454,共6页China Pharmacist

摘　　要：目的:建立高效分子排阻色谱法(Cef-SEC)测定注射用盐酸头孢吡肟中的多聚体杂质,并应用在线脱盐-高效液相色谱-离子阱-飞行时间质谱联用技术(2D-LC-IT-TOF-MS/MS)对检出的四个杂质进行鉴定。方法:色谱柱:SRT-Cef-SEC(300 mm×7.8 mm, 5μm);流动相:5 mmol·L^(-1)磷酸盐缓冲液-乙腈(98∶2);进样量:20μl;检测波长:254 nm;ESI离子源,正离子扫描;主成分自身对照法计算多聚体杂质的含量。结果:在该条件下,盐酸头孢吡肟峰与前后杂质峰分离良好;在0.5~50.0μg·ml;浓度范围内,样品浓度与多聚体杂质峰面积呈良好线性关系(r=0.999 9);检出限(LOQ)为5 ng;检测限为(LOD)2 ng。结论:本方法简便、准确、灵敏、可靠,可有效检测盐酸头孢吡肟中多聚体杂质的含量。Objective: To establish a high performance size exclusion chromatography(Cef-SEC) method for determining the polymer impurities in cefepime hydrochloride for injection and identify their structure by 2 D-LC-IT-TOF-MS/MS. Methods: The analysis was carried out by using a STR-Cef-SEC chromatography column(300 mm×7.8 mm). The mobile phase was 5 mmol·L;ammonium acetate and acetonitrile(95∶5). The detection wavelength was 254 nm. The injection volume was 20 μl. The ion source was ESI ionization source, the scan pattern was positive and the contents of the polymers were determined by main component self-compare without calibration factor. Results: The polymers were completely separated from cefepime hydrochloride. The calibration curves were linear within the range of 0.5-50.0 μg·ml^(-1) for cefepime hydrochloride(r=0.999 9). The LOQ was 5 ng for cefepime hydrochloride. The LOD was 2 ng for cefepime hydrochloride. Conclusion: The method provides basis for the separation and analysis of the polymers in cefepime hydrochloride for injection, and can be used to improve the quality of the product.

关 键 词：盐酸头孢吡肟 多聚体杂质 高效分子排阻色谱法 在线脱盐-高效液相色谱-离子阱-飞行时间质谱 

分 类 号：TQ460.72[医药卫生—药物分析学]