HPLCMS法鉴定左氧氟沙星的降解产物.pdfVIP

498 药学学报 Acta Pharmaceutica Sinica 2012, 47 (4) : 498 501 HPLC-MS 鉴定左氧氟沙星的降解产物 王维剑, 李 涛, 李 军, 刘 琦, 谢元超* ( 山东省食品药品检验所, 山东 济南 250101) 摘要: 采用高效液相色谱-质谱联用法 (HPLC-MS) 鉴定左氧氟沙星的降解产物。以 Agilent ZORBAX Extend-C18 (250 mm × 4.6 mm, 5 μm) 色谱柱为分析柱, 0.1%醋酸铵溶液 (用甲酸调节至pH 3.5) 乙腈为流动相, 梯度洗脱, 流速为0.5 mL·min 1, 柱温为40 ℃。通过与对照品比较, 结合质谱仪扫描结果分析, 在左氧氟沙星的 破坏样品中检测出去羧基左氧氟沙星 (m/z 318.2) 、去甲基左氧氟沙星 (m/z 348.3)、左氧氟沙星-N -氧化物 (m/z 378.1) 等降解产物。本方法简单可行, 结果准确可 , 可用于左氧氟沙星降解产物的定性鉴别。 关键词: HPLC-MS; 左氧氟沙星; 降解产物 中图分类号: R917 文献标识码:A 文章编号: 05 13-4870 (2012) 04-0498-04 HPLC-MS identification of degradation products of levofloxacin * WANG Wei-ji an, LI Tao, LI Jun, LIU Qi, XIE Yuan-chao (Shandong Provincial Institute for Food and Drug Control, Jinan 250101, China) Abstract: The study aims to identify the degradation products of levofloxacin by HPLC-MS. The degradation products of levofloxacin were chromatographed on Agilent Zorbax Extend-C 18 column (250 mm × 4.6 mm, 5 μm). The mobile phase was 0.1% ammonium acetate solution (using methanoic acid to adjust to pH 3.5)- acetonitrile at the flow rate of 0.5 mL·min 1 (gradient elution), the column temperature was 40 ℃. Descarboxyl levofloxacin, desmethyl levofloxacin and levofloxacin N-oxide were identified through comparing with the standard spectrum and the results of mass spectrometry, i.e. m/z 318.2 was descarboxyl levofloxacin, m/z 348.2 was desmethyl levofloxacin, m/z 378.1 was levofloxacin-N -oxide. This method is simple, f