| 引用本文: | 袁红露,朱程玉,李伟举,杨荷友,黄梅,周雪飞.离子色谱-抑制电导检测法测定环磷酰胺相关物质A的含量[J].中国现代应用药学,2014,31(5):567-570. |
| YUAN Honglu,ZHU Chengyu,LI Weiju,YANG Heyou,HUANG Mei,ZHOU Xuefei.Determination of Cyclophosphamide Related Substance A by Ion Chromatography-Suppressed Conductivity Detection[J].Chin J Mod Appl Pharm(中国现代应用药学),2014,31(5):567-570. |
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| 摘要: |
| 目的 采用离子色谱-抑制电导检测法测定环磷酰胺相关物质A的含量。方法 采用色谱柱lonPac CS12A (250 mm×4.0 mm Analytical)，以0.16%甲烷磺酸为流动相，流速为1.0 mL·min-1，检测器为电导检测器，柱温为25 ℃，进样量为25 μL。结果 环磷酰胺相关物质A的定量下限为1.8 μg·mL-1，检测限为0.54 μg·mL-1；在1.8~24 μg·mL-1内线性关系良好(r>0.999)，在不同浓度水平范围内的平均回收率为97.45%~99.81%，RSD<3%。结论 本方法选择性好，灵敏度高，结果可靠，可满足环磷酰胺相关物质A检验分析的需要。 |
| 关键词: 离子色谱法 抑制电导检测法 环磷酰胺 相关物质A |
| DOI： |
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| 基金项目:国家自然科学基金(20936005) |
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| Determination of Cyclophosphamide Related Substance A by Ion Chromatography-Suppressed Conductivity Detection |
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YUAN Honglu1,2, ZHU Chengyu1,2, LI Weiju2, YANG Heyou2, HUANG Mei1, ZHOU Xuefei2
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1.Department of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310058, China;2.Zhejiang Hisun Pharmaceutical Co., Ltd., Taizhou 318001, China
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| Abstract: |
| OBJECTIVE To establish ion exchange chromatography-suppressed conductivity detection for the determination of related substance A in cyclophosphamide. METHODS Using a Ionpac CS12A column (250 mm×4.0 mm Analytical), the mobile phase was 0.16% methane sulfonic acid, the flow rate was 1.0 mL·min-1 with suppressed conductivity detector; the column temperature was 25 ℃; and the inject volume was 25 μL. RESULTS The detection and quantification limit was 0.54 and 1.8 μg·mL-1, respectively. The linear range for the content of degradation impurity A was 1.8-24 μg·mL-1(r>0.999), the average recoveries were in the range of 97.45%-99.81% with the relative standard deviation below 3%. CONCLUSION The method is simple, rapid, accurate and is suitable for the determination of cyclophosphamide degradation impurity A. |
| Key words: ion chromatography suppressed conductivity detection cyclophosphamide related substance A |
