依诺沙星制剂有关物质的研究

发布时间：2018-12-11 10:00

【摘要】：目的:采用高效液相色谱-三重串联四极杆质谱及超高分辨四极杆傅里叶变换离子回旋共振串联质谱仪对依诺沙星主要有关物质进行结构鉴定。方法:采用高效液相色谱法测定75批依诺沙星制剂中的有关物质,确定含量不低于0.1%的主要杂质。采用Thermo Accucore XL C18色谱柱(4.6 mm×250 mm,4μm)及高效液相色谱-三重串联四极杆质谱,以0.1%甲酸溶液(含5 mmol·L~(-1)醋酸铵)-甲醇-乙腈(86∶5∶9)为流动相A,以0.1%甲酸溶液(含5 mmol·L~(-1)醋酸铵)-甲醇-乙腈(350∶325∶325)为流动相B进行梯度洗脱,对依诺沙星有关物质进行分离,并初步测定主要有关物质准分子离子质荷比;采用傅里叶变换质谱法测定有关物质准确母离子及子离子,并结合对照品及裂解规律,对主要有关物质进行结构推定。结果:在所建立的高效液相色谱-三重串联四极杆质谱条件下,依诺沙星及其有关物质可达到良好分离。依诺沙星制剂中3个主要有关物质均具有依诺沙星的1,8-萘啶母核结构。结论:本研究对依诺沙星制剂中的主要有关物质进行了结构鉴定,为改进生产工艺和提高产品质量提供了参考依据。
[Abstract]:Aim: to identify the main related substances of enoxacin by high performance liquid chromatography-triple tandem quadrupole mass spectrometry and ultrahigh resolution quadrupole Fourier transform ion cyclotron resonance mass spectrometer. Methods: the related substances in 75 batches of enoxacin preparations were determined by HPLC, and the main impurity of above 0.1% was determined. Thermo Accucore XL C18 column (4.6 mm 脳 250 mm,4 渭 m) and high performance liquid chromatography-triplex tandem quadrupole mass spectrometry (HPLC-MS) were used. The mobile phase A was 0.1% formic acid solution (containing 5 mmol L ~ (-1) ammonium acetate) -methanol-acetonitrile (86:5:9). The related substances of enoxacin were separated by gradient elution with 0.1% formic acid solution (containing 5 mmol L ~ (-1) ammonium acetate) -methanol-acetonitrile (350: 325: 325) as mobile phase B. The excimer ion charge ratio of the main related substances was preliminarily determined. The method of Fourier transform mass spectrometry (FTMS) was used to determine the accurate parent ions and sub-ions of the related substances, and the structure of the main related substances was deduced by combining the reference substance and the law of cracking. Results: Enofloxacin and its related substances could be separated well under the conditions of high performance liquid chromatography-triple tandem quadrupole mass spectrometry. The three main related substances in enoxacin preparation all have the nuclear structure of 1 ~ 8-Naphthyridine of enrofloxacin. Conclusion: in this study, the main related substances in enoxacin preparation were identified, which provided a reference for improving the production process and product quality.
【作者单位】：厦门市药品检验所;
【分类号】：R927.1

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