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HPLC-MS法鉴定左氧氟沙星的降解产物
作者姓名:Wang WJ  Li T  Li J  Liu Q  Xie YC
作者单位:山东省食品药品检验所
基金项目:国家科技重大专项课题-重大新药创制资助项目(2009ZX09313-023)
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,5μm)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,结果准确可靠,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

HPLC-MS identification of degradation products of levofloxacin
Wang WJ,Li T,Li J,Liu Q,Xie YC.HPLC-MS identification of degradation products of levofloxacin[J].Acta Pharmaceutica Sinica,2012,47(4):498-501.
Authors:Wang Wei-Jian  Li Tao  Li Jun  Liu Qi  Xie Yuan-Chao
Institution: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-C18 column (250 mm x 4.6 mm, 5 microm). 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 x min(-1) (gradient elution), the column temperature was 40 degrees C. 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, fast, accurate and suitable for the identification of degradation products of levofloxacin.
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