期刊文献+

FMOC柱前衍生化HPLC法测定阿仑膦酸钠片含量及有关物质4-氨基丁酸 被引量:10

Determination of Alendronate Sodium Tablets and Its Related Substances 4-Aminobutyric by HPLC Pre-column Derivatization with FMOC
下载PDF
导出
摘要 目的建立9-氯甲酸芴甲酯(FMOC)柱前衍生化高效液相色谱法测定阿仑膦酸钠片的含量及其有关物质4-氨基丁酸。方法碱性条件下供试品与FMOC衍生化反应,采用ODS-2HYPERSILC18色谱柱,乙腈-0.4%EDTA(pH=7.2)(35∶65)为流动相,测定阿仑膦酸钠的衍生化产物;以乙腈-0.4%EDTA(pH=7.2)(40∶60)为流动相,测定4-氨基丁酸衍生化产物,紫外检测器(λ=265nm),荧光检测器(λex=260nm,λem=310nm)。结果阿仑膦酸钠浓度在10~60μg·mL-1范围内(UV265nm)线性关系良好(r=0.9996);平均回收率100.3%(n=9)。有关物质4-氨基丁酸浓度在1~5μg·mL-1范围内(UV265nm)线性关系良好(r=0.9998)。结论本方法简单、准确、灵敏。 Objective A HPLC method with pre-column derivatization has been developed for test of related substances 4-aminobutyric and determination of Alendronate Sodium Tablets.Methods Alendronate sodium was derivatized with 9-fluorenylmethyl chloroformate(FMOC)in 0.05mol Na2CO3 solution,the analytical column was ODS-2 HYPERSIL C18,acetonitrile-0.4%EDTA(pH7.2)(35∶65)as mobile phase for alendronate sodium and acetonitrile-0.4%EDTA(pH7.2)(35∶65)as mobile phase for 4-aminobutyric acid,UV detection at 265nm;FLD λex=260nm, λem= 310nm. Results Alendronate sodium was linear at the concentration range of 10~60μg·mL^-1 (UV265nm; r= 0. 9996) and 4-aminobutyric acid was linear at the concentration range of 1μg·mL^-1 (UV265nm;r=0. 9998). The average recovery rate of alendronate sodium was 100. 3%(n=9). Conclusions The method is sample, accurate and sensitive.
作者 楼永明
出处 《中国药事》 CAS 2009年第10期974-977,共4页 Chinese Pharmaceutical Affairs
关键词 阿仑膦酸钠 4-氨基丁酸 柱前衍生化 高效液相色谱法 alendronate sodium 4-aminobutyric acid pre-column derivatization HPLC
  • 相关文献

参考文献7

二级参考文献99

  • 1张晓青,蒋晔,徐智儒.唑来膦酸及其有关化合物的反相离子对高效液相色谱分离[J].色谱,2004,22(4):428-430. 被引量:3
  • 2邓海根,曹雨震.高效液相色谱仪的通用型质量检测器──蒸发光散射检测器(ELSD)[J].药物分析杂志,1994,14(3):61-63. 被引量:56
  • 3中华人民共和国药典委员会.中国药典(二部)[S].2000年版[M].北京:化学工业出版社,2000.附录XIE:86,204.
  • 4Spackman D H, Stein W H, Moore S. Anal. Chem., 1958, 30(7): 1190~1206.
  • 5Wiedmeijer V T, Porterfield S P, Hendrich C E. J. Chromatogr., 1982, 231: 410~417.
  • 6McClung G, Frankenberger Jr W T. J. Liq. Chromatogr., 1988, 11(3): 613~646.
  • 7Fürst P, Pollack L, Graser T A, Godel H , Stehle P. J. Chromatogr., 1990, 499: 557~569.
  • 8Morton R C, Gerber G E. Anal. Biochem., 1988, 170: 220~227.
  • 9Kochbar S, Christen P. Anal. Biochem., 1989, 178: 17~21.
  • 10Fermo I, Vecchi E D E, Diomede L, Paroni R. J. Chromatogr., 1990, 534: 23~35.

共引文献155

同被引文献97

引证文献10

二级引证文献55

相关作者

内容加载中请稍等...

相关机构

内容加载中请稍等...

相关主题

内容加载中请稍等...

浏览历史

内容加载中请稍等...
;
使用帮助 返回顶部