HPLC-CAD法测定硫酸卡那霉素中的硫酸盐含量  

Determination of Sulfate Contents in Kanamycin Sulfate by HPLC-CAD Method

作　　者：李珉 侯金凤 陆岩[1] 车宝泉[1] 王俊秋[1] 李文东[1] LI Min;HOu Jin-feng;LU Yan;CHE Bao-quan;WANG Jun-qiu;LI Wen-dong(Beijing Institute of Drug Control,NMPA Key Laboratory for Researeh and Evaluation of GenericDrugs,Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine,Beijing 102206,China)

机构地区：[1]北京市药品检验所,国家药品监督管理局仿制药研究与评价重点实验室,中药成分分析与生物评价北京市重点实验室,102206

出　　处：《首都食品与医药》2021年第4期172-174,共3页Capital Food Medicine

摘　　要：目的建立测定硫酸卡那霉素原料中硫酸盐含量的高效液相色谱-电喷雾检测器(HPLC-CAD)方法.方法采用Waters HSS T3色谱柱(4.6mm×250mm,5μm),以0.2mol/L三氟乙酸水溶液为流动相,流速0.3mL·min^(-1),柱温30℃,电喷雾检测器的喷雾器温度为35℃.结果采用新建方法,硫酸盐与亚硫酸盐、卡那霉素及其有关物质分离情况良好,硫酸盐在0.038mg/mL~0.15mg/mL范围内浓度与峰面积线性关系良好(r>0.999),检出限可达到0.08μg.结论新建的方法较现行标准方法专属性好、灵敏度高,可以满足硫酸卡那霉素原料中硫酸盐含量测定的分析要求.0bjective To establish a high performance liquid chromatography-charged aerosol detector(HPLC-CAD)method for the determination of the sulfate contents in kanamycin sulfale raw materials.Methods A Walers HSS T3 column(4.6mm×250mm,5μm)was used.A n aqueous solution,containing 0.2mol/L trifluoroacetate,was used as the mobile phase.The flow rate was 0.3mL·min^(-1),and the column temperature was 30℃.The spray temperature of CAD was 35Ti.Results By using this novel method,sulfate,sulfite,ka namycin and related substances were well separated.The linear relationship between sulfate concentration and peak area was in the range of 0.038m g/m L~0.15m g/mL(r>0.999).The limit of detection could reach 0.08μg.Conclusion Comparing with the current standard method,the sensitivity and the separation capacity of this novel method are much better,which can detect more impurities and meet the analysis requirements of related substances,sulfate and kanamycin content in kanamycin sulfate raw materials and its injection.

关 键 词：电喷雾检测器 硫酸卡那霉素 单硫酸卡那霉素 硫酸盐测定 氨基糖苷类抗生素 高效液相色谱法 

分 类 号：R927.2[医药卫生—药学]