注射用头孢噻肟钠有关物质测定法中色谱参数转化的探讨  

Discussion on transformation of chromatographic parameters in determination of related substances of Cefotaxime Sodium for Injection

作　　者：李婕[1] 陈丽莉 徐子航 徐永威 曹媛媛 黄海伟[1] LI Jie;CHEN Lili;XU Zihang;XU Yongwei;CAO Yuanyuan;HUANG Haiwei(National Institutes for Food and Drug Control,Beijing 102269,China;Shanghai Xinya Pharmaceutical Co.,Ltd.,Shanghai 201209,China;Waters Technology(Shanghai)Co.,Ltd.,Shanghai 201206,China)

机构地区：[1]中国食品药品检定研究院,北京102269 [2]上海上药新亚药业有限公司,上海201209 [3]沃特世科技(上海)有限公司,上海201206

出　　处：《药物评价研究》2022年第7期1350-1354,共5页Drug Evaluation Research

摘　　要：目的将《中国药典》项下注射用头孢噻肟钠有关物质测定法的色谱参数进行转化,缩短液相分析时间,提高检测效率。方法采用Waters Xselect HSS T3 C_(18)柱(100 mm×3 mm,2.5μm)色谱柱,流动相A为0.05 mol·L^(−1)磷酸盐缓冲液(pH 6.25)-甲醇(86∶14),流动相B为0.05 mol·L^(−1)磷酸盐缓冲液(pH 6.25)-甲醇(60∶40),先以流动相A-流动相B(95∶5)等度洗脱,待头孢噻肟钠洗脱完毕后,立即进行线性梯度洗脱(0~0.7 min 95%→75%A,0.7~2.7 min 75%A,2.7~7.8min 75%→0A,7.8~9.5min 100%B,9.5~11.2min 0→95%A,11.2~14.6min 95%A),体积流量为0.5mL·min^(−1),进样体积为2μL,检测波长为235 nm。结果色谱参数转化后运行时间从80 min缩短至26 min,方法专属性、稳定性、色谱柱耐用性均良好。结论色谱参数转化后的方法专属、节能环保,可用于注射用头孢噻肟钠的有关物质检测。Objective Transformation of chromatographic parameters in determination of related substances of Cefotaxime Sodium for Injection in chinese pharmacopoeia to shorten the analysis time and improve the efficiency.Methods Waters Xselect HSS T3 C_(18)(100 mm×3 mm,2.5μm)was adopted with 0.05 mol·L^(−1)phosphate buffer(pH 6.25)-methanol(86∶14)as mobile phase A,0.05 mol·L^(−1)phosphate buffer(pH 6.25)-methanol(60∶40)as mobile phase B.The mobile phase A and B(95∶5)were used for constant elution.After the elution of cefotaxime sodium,linear gradient elution was performed immediately(0—0.7 min 95%→75%A,0.7—2.7 min 75%A,2.7—7.8 min 75%→0 A,7.8—9.5 min 100%B,9.5—11.2 min 0 A→95%A,11.2—14.6 min 95%A),the flow rate was 0.5 mL·min^(−1),the injection volume was 2μL,and the detection wavelength was 235 nm.Results After the conversion of chromatographic parameters,the running time was reduced from 80 min to 26 min,and the specificity,stability and durability of chromatographic column were good.Conclusion The method after the transformation of chromatographic parameters is rapid,exclusive,energy saving and environmental protection.It can be used for the determination of related substances of Cefotaxime Sodium for Injection.

关 键 词：注射用头孢噻肟钠 有关物质 高效液相色谱 色谱参数 转化 

分 类 号：R917[医药卫生—药物分析学]