摘要
目的采用LC/MSn技术推断拉氧头孢钠原料中杂质的结构。方法采用Shiseido TYPE UG80C18(4.6mm×250mm,5μm)色谱柱,以0.01mol/L醋酸铵溶液-甲醇(99:1,V/V)作为流动相A,以0.01mol/L醋酸铵溶液-甲醇(70:30,V/V)为流动相B,进行梯度洗脱分离杂质。通过强力试验归属杂质的来源,在正离子模式下获取各杂质的质谱数据,结合头孢菌素的普遍质谱裂解规律和降解反应原理,解析相关杂质的结构。结果推断了12种杂质的化学结构,样品中未检出聚合物杂质。结论LC/MSn法可快速准确推断拉氧头孢钠原料中杂质结构,中国药典的拉氧头孢钠质量标准需要进一步提高。
Objective To characterize the impurity structures in latamoxef sodium raw material. Methods Impurities were eluted gradiently on a Shiseido UG80 C18 column, with 0.01mol/L ammonium acetate solutionmethanol (99:1, V/V) as mobile phase A, and 0.01mol/L ammonium acetate solution-methanol (70:30, V/V) as mobile phase B. Stress tests were designed and performed on the raw material to specify those impurities. By application of the on-line LC/MSn method, the impurities were analyzed in a positive mode and their structures were characterized based on the degradation mechanism and mass fragmentation regularity of cephalosporin. Results A total of 12 impurities were characterized in the raw material including four degradation products and eight impurities derived from the synthesis process, but no polymer impurities were detected. Conclusion The structures of related impurities in latamoxef lodium raw material can be rapidly identified by the on-line LC/MSn method, and the specification of latamoxef sodium raw material in China Pharmacopeia should be further optimized and improved.
作者
李进
姚尚辰
胡昌勤
Li Jin;Yao Shang-chen;Hu Chang-qin(National Institute for Food and Drug Control, Beijing 102629)
出处
《中国抗生素杂志》
CAS
CSCD
2019年第7期820-833,共14页
Chinese Journal of Antibiotics
