高效液相色谱法测定创新药物N^1,N^2-双(2,3-二羟基-4,6-二磺酸苄基)亚乙基二胺钠盐的含量  

Determination of a new drug N^1,N^2-bis (2,3-dihydroxy-4,6-disulfonic acid benzyl) ethylenediamine sodium salt by HPLC

作　　者：王若琪 高洁 刘欢[1] 尹晶晶[1] 胡波[2] 李建国[1] WANG Ruo-qi;GAO Jie;LIU Huan;YIN Jing-jing;HU Bo;LI Jian-guo(Drug Safety Evaluation Center of China Institute for Radiation Protection,Shanxi Key Laboratory of Drug Toxicology and Drug for Radiation Injury,CNNC Key Laboratory on Radiotoxicology and Radiopharmaceutical Preclinical Evaluation,Taiyuan 030006;Irradiation Technology Center of China Institute for Radiation Protection,Taiyuan 030006)

机构地区：[1]中国辐射防护研究院,药物毒理与放射损伤药物山西省重点实验室,中核放射毒理与放射性药物临床前评价重点实验室,太原030006 [2]中国辐射防护研究院辐照技术中心,太原030006

出　　处：《中南药学》2020年第8期1365-1369,共5页Central South Pharmacy

基　　金：乏燃料后处理科研专项基金(No.HC17110217)。

摘　　要：目的建立HPLC法测定重金属促排药物N1,N2-双(2,3-二羟基-4,6-二磺酸苄基)亚乙基二胺钠盐(NBED)的含量。方法采用RP-HPLC法,色谱柱为Waters Symmetry C18柱(4.6 mm×250 mm,5 μm),以磷酸盐缓冲液(10 mmol·L-1磷酸二氢钾、10 mmol·L-1四丁基溴化铵,磷酸调pH至2.5)-乙腈(90∶10)为流动相,流速0.8 mL·min-1,检测波长212 nm,柱温30℃,进样量10 μL。结果 NBED在4.12~41.16 μg·mL-1与峰面积线性关系良好(r=1.000)。NBED主成分与有关物质分离度良好,主峰纯度良好,破坏试验产生的降解杂质对NBED的定量分析均不产生干扰。平均回收率为99.5%~101.9%(n=3)。结论所建方法专属性强,灵敏度高,准确可靠,适用于NBED原料药的质量控制。Objective To determine the content of N1,N2-bis (2,3-dihydroxy-4,6-disulfonic acid benzyl) ethylenediamine sodium salt (NBED) by HPLC.Methods RP-HPLC was adopted to determine NBED with a Waters Symmetry C18 column (4.6 mm×250 mm,5 μm).Phosphate buffer solution (10 mmol·L-1 potassium dihydrogen phosphate,10 mmol·L-1 tetrabutylammonium bromide,and pH being adjusted to 2.5)-acetonitrile (90∶10,v/v) was used as the mobile phase.The detection wavelength was 212 nm,the flow rate was 0.8 mL·min-1,the column temperature was 30℃,and the injection volume was 10 μL.Results Under the above chromatographic conditions,the linear range of NBED was 4.12~41.16 μg·mL-1 (r=1.000).Related substances were seperated from NBED,and the purity of the main peak was good.The degradation impurities generated by the destruction test didn’t interfere with the determination of the main peak.The average recovery was 99.5%~101.9% (n=3).Conclusion The method is specific,sensitive,accurate and reliable,which can be used in the quality control of NBED raw material.

关 键 词：NBED原料药 有关物质 含量测定 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]