高级检索

    UHPLC-HRMS定量检测莫西沙星中5种亚硝胺类化合物

    Quantitative Determination of 5 Nitrosamines in Moxifloxacin by UHPLC-HRMS

      摘要
    • 摘要: 目的 基于超高效液相色谱和高分辨质谱建立同时检测莫西沙星中5种亚硝胺类基因毒性杂质的定量分析方法。方法 采用ACE Excel 1.7 C18-PFP(100 mm×2.1 mm，1.7 μm)色谱柱，0.1%甲酸水-甲醇为流动相，0.3 mL·min-1的流速进行梯度洗脱。采用四极杆高分辨静电场轨道阱质谱在电喷雾正离子条件下运用平行反应监测模式对5种亚硝胺类化合物进行定量检测。结果 5种亚硝胺类基因毒性杂质的定量限均≤0.5 ng·mL-1。NPYP、NEMA和NDEA的标准曲线在1.0~100 ng·mL-1(NPIP和NDBA为0.1~100 ng·mL-1)呈良好线性关系(R2≥0.998)。该方法在盐酸莫西沙星药物中的回收率为93.1%~114.1%，RSD为0.7%~4.6%。结论 本方法结果准确、灵敏度高、重复性好，适用于盐酸莫西沙星中亚硝胺类基因毒性杂质的含量检测。

       

      Abstract: OBJECTIVE To develop and validate a UHPLC/HRMS method for simultaneous quantitation of 5 genotoxic nitrosamines in moxifloxacin.METHODS ACE Excel 1.7 C18-PFP(100 mm×2.1 mm, 1.7 μm) column was used, separated by gradient elusion using a mixture of water and methanol with 0.1% formic acid at 0.3 mL·min-1, and 5 nitrosamines were detected by parallel reaction monitoring using Q Exactive mass spectrometer in electrospray positive mode.RESULTS The lower limits of quantitation for 5 genotoxic nitrosamines ≤0.5 ng·mL-1. Good linearity was established for NPYR, NEMA and NDEA over 1.0-100 ng·mL-1, and for NPIP and NDBA over 0.1-100 ng·mL-1(R2≥0.998), respectively. The intra-assay accuracy of 5 nitrosamines in moxifloxacin hydrochloride was determined to be from 93.1% to 114.1%, and the RSD was found to be from 0.7% to 4.6%.CONCLUSION The validated method provides satisfactory sensitivity and specificity for analysis of genotoxic nitrosamines as impurities in moxifloxacin hydrochloride.

       

      • HTML全文
      • 参考文献(18)
      • 相关文章
      • 施引文献
    • 资源附件(0)

    /

    返回文章
    返回