HPLC-ECD法测定盐酸大观霉素有关物质  

Determination of spectinomycin hydrochloride related substances by HPLC-ECD

作　　者：周桂云 陈平 孙秀丽 王晓茹 郭丽 王梅 

机构地区：[1]山东鲁抗医药股份有限公司,济宁272120

出　　处：《药物分析杂志》2012年第9期1665-1668,1672,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立HPLC-ECD法测定盐酸大观霉素有关物质。方法:应用高效液相色谱-电化学检测器,Waters XBridge C18色谱柱(4.6 mm×250 mm,5μm),以pH 3.2的草酸盐缓冲溶液-乙腈(1000∶105)为流动相,流速为1.0 mL.min-1;柱后溶液为21 g.L-1的氢氧化钠溶液,流速0.5 mL.min-1;ECD系统参数:极性为阳性,检波+0.12 V,氧化电位+0.70 V,还原电位-0.60 V,范围20μA。结果:盐酸大观霉素有关物质在2.25～45μg.mL-1范围内呈良好的线性关系,r=0.9999;Y轴截距在100%浓度响应值的7.3%处,在100%浓度的25%～500%的范围内,对任一点的响应值在此点理论值的97.7%至103.6%的范围内;平均回收率(n=9)为98.9%,RSD为2.9%。结论:该方法简便易行,准确度高,重复性好,可用于盐酸大观霉素及相关制剂产品的质量控制。Objective：To establish a quantitative method for spectinomycin hydrochloride related substances by HPLC -ECD. Methods：The detection was performed on a Waters XBridge C1 column （4. 6 mm - 250mm,5μm）. The mobile phase was a mixture of pH 3.2 oxalate buffer and acetonitrile in a ratio of 1000：105 ,with a flow rate of 1.0 mL - min -1 ;The post - column derivatization solution was 21 g · L-1 sodium hydroxide solution with a flow rate of 0. 5 mL ·min 1. ECD system parameters ： Polarity ： Positive ; Detector ： ＋ 0. 12 V ; Oxidation potential ： ＋ 0.70 V ; Reduction potential ： - O. 60 V ; Range ： 20 μA. Results： The linear range of the spectinomycin hydrochloride related substances was 2.25 -45 μg mL-l ,the correlation coefficient was 0. 9999. Y axial intercept in 100% concentra- tion response valve is 7.3% ,in 100% the concentration of 25% -500% range,the response value of any point ranged from 97.7% to 103.6% of the theoretical value. The average recovery rate（ n = 9）was 98.9%, RSD was 2.9%. Conclusion：The method is simple, reliable, accurate and reproducible, which can be used for the quality control of spectinomycin hydrochloride and related finished products.

关 键 词：高效液相色谱-电化学检测 氨基糖苷类抗生素 盐酸大观霉素 有关物质结构推测 杂质含量测定 

分 类 号：R917[医药卫生—药物分析学]