硫酸核糖霉素分子式中硫酸数目的确定及控制方法的比较  

Determine the Number of Sulfate in the Formula of Ribostamycin Sulphate and Select a Suitable Method to Control Its Sulphate Content

作　　者：耿悦 张如梦 侯玉荣 施海蔚 张锦琳 潘广文 柳文媛[2] 袁耀佐 GENG Yue;ZHANG Rumeng;HOU Yurong;SHI Haiwei;ZHANG Jinlin;PAN Guangwen;LIU Wenyuan;YUAN Yaozuo(Jiangsu Institute for Food and Drug Control,Nanjing 210019,China;Key Laboratory of Drug Quality Control and Pharmacovigilance(China Pharmaceutical University),Ministry of Education,Nanjing 210009,China;Thermo Fisher Science and Technology(China)Co.Ltd.,Shanghai 201203,China)

机构地区：[1]江苏省食品药品监督检验研究院,南京210019 [2]药物质量与安全预警教育部重点实验室(中国药科大学),南京210009 [3]赛默飞世尔科技(中国)有限公司,上海201203

出　　处：《药学与临床研究》2018年第6期417-421,共5页Pharmaceutical and Clinical Research

基　　金：国家重大新药创制-化药制剂质量评价关键技术研究课题(2015ZX09303001);2017年国家评价性抽验品种

摘　　要：目的:为了确定硫酸核糖霉素分子式中硫酸的数目,并选择适合的方法控制其硫酸盐的含量。方法:建立了高效液相色谱-蒸发光散射法(HPLC-ELSD)对硫酸核糖霉素的硫酸盐(SO4)含量进行测定,并开发出了同样适用的离子色谱电导法(HPIC-CD)进行结果比对。同时采用《中国药典》方法测定硫酸核糖霉素的酸碱度。结果:HPLC-ELSD法,硫酸盐(SO4)在15～250μg·mL-1范围内线性良好,检测限和定量限分别为0.16μg和0.25μg,回收率为101.1%;HPIC-CD法,硫酸盐(SO4)在20～180μg·mL-1范围内线性良好,检测限和定量限分别为0.17 ng和0.50 ng,回收率为99.8%。结论:两种硫酸盐测定方法,专属性强,灵敏度高,重复性好,测定结果无显著性差异,分子式中硫酸的数目约为1.5,进一步发现,硫酸盐含量和溶液pH值呈显著负相关,并具有一定的线性关系,酸碱度检查可以控制硫酸盐的含量。Objective:In order to determine the number of sulphate in the formula of ribostamycin sulphate and select a suitable method to control its sulphate content.Methods:An high performance liquid chromatography-evaporative light scattering detection method(HPLC-ELSD)was established to determine the sulfate content,and an applicable ion chromatography conductance detection method(HPIC-CD)was also developed for comparison.At the same time,the pharmacopeia method was used to determine the acidity or alkalinity of ribostamycin sulphate.Result:HPLC-ELSD method showed good linearity of sulfate(SO4)in the range of 15-250μg·mL^-1.The LOD and LOQ were respectively 0.16μg and 0.25μg,the recovery was 101.1%.The HPIC-CD method showed good linearity of sulfate(SO4)in the range of 20-180μg·mL^-1.The LOD and LOQ were respectively 0.17 ng and 0.50 ng,the recovery was 99.8%.Conclusion:The two established methods show strong specificity,high sensitivity and good repeatability.The test results show no significant difference between the two methods.The number of sulfate in the molecular formula was about 1.5.It was further found that the sulfate content was significantly negatively correlated with the pH value of the solution and had certain linear relationship.The acidity or alkalinity test can be used to control the content of sulfate.

关 键 词：高效液相色谱蒸发光散射法 离子色谱电导法 硫酸盐 硫酸核糖霉素 

分 类 号：R927[医药卫生—药学]