色谱 ›› 2012, Vol. 30 ›› Issue (12): 1292-1294.DOI: 10.3724/SP.J.1123.2012.08044

• 技术与应用 • 上一篇    下一篇

反相离子对色谱法测定脱氧精胍菌素药物中的主成分

程晓昆, 王娅莉, 张惠敏, 牛长群*   

  1. 华北制药集团新药研究开发有限责任公司, 河北 石家庄 050015
  • 收稿日期:2012-08-24 修回日期:2012-10-08 出版日期:2012-12-28 发布日期:2012-12-19
  • 通讯作者: 牛长群,正高级工程师,主要从事新药研究开发工作. Tel: (0311)86993040, E-mail: niuchangqun@126.com.

Determination of a major constituent in deoxyspergualin drug by reversed-phase ion-pair chromatography

CHENG Xiaokun, WANG Yali, ZHANG Huimin, NIU Changqun*   

  1. North China Pharmaceutical Group New Drug Research and Development Co., Ltd, Shijiazhuang 050015, China
  • Received:2012-08-24 Revised:2012-10-08 Online:2012-12-28 Published:2012-12-19

摘要: 建立了反相离子对色谱法分离测定脱氧精胍菌素药物中主成分的方法。分别考察了色谱柱类型、离子对试剂种类及浓度、缓冲盐浓度和流动相pH值等参数对实验结果的影响。确定了分离脱氧精胍菌素的最佳条件: C18色谱柱(250 mm×4.6 mm, 5 μm);以5 mmol/L磷酸氢二钾水溶液(含5 mmol/L戊烷磺酸钠,pH 3.6±0.3)-乙腈(90:10, v/v)为流动相,流速为1.0 mL/min;检测波长为210 nm;柱温为30 ℃;进样量为20 μL。该方法实现了对脱氧精胍菌素的良好分离,且线性关系良好,检出限可达0.5 mg/L。

关键词: 反相高效液相色谱法, 离子对试剂, 脱氧精胍菌素, 药物

Abstract: A method was established for the determination of deoxyspergualin using reversed-phase ion-pair chromatography (RP-IPC). Several parameters, such as the chromatographic column, the types and concentration of ion-pair reagents, the concentration of the buffer and the pH value of the mobile phase were evaluated. The optimal separation conditions were as follows: C18 column (250 mm×4.6 mm, 5 μm); mobile phase, 5 mmol/L di-potassium hydrogen phosphate (containing 5 mmol/L 1-pentanesulfonic acid sodium, pH 3.6±0.3)-acetonitrile (90:10, v/v); flow rate, 1.0 mL/min; detection wavelength, 210 nm; column temperature, 30 ℃; injection volume, 20 μL. Under the optimaized experimental conditions, good linear relationships was obtained and the limit of detection for deoxyspergualin was 0.5mg/L.

Key words: deoxyspergualin (DSG), drug, ion-pair reagents, reversed-phase ion-pair chromatography (RP-IPC)