注射用头孢他啶中吡啶的检测方法研究

摘要

目的：对注射用头孢他啶中吡啶的检测方法进行研究，为提高该药质量标准、临床配制使用、合理包装贮存及说明书修订等提供参考。方法采用高效液相色谱（HPLC）法，外标以吡啶含量为指标，进行检测方法的线性关系试验、精密度试验及稳定性试验；对样品进行1个月加速试验、影响因素试验，比较该条件下产品质量；对按产品使用说明书中的配制方法配制样品溶液进行稳定性试验，比较头孢他啶中吡啶在不同配制溶液中的含量变化。结果吡啶线性回归方程为Y=168580X-2451，R2=0.9998，在0.0552~0.6619μg内与峰面积线性关系良好；精密度试验吡啶色谱峰面积相对标准偏差（RSD）为0.29%；稳定性试验下，新旧吡啶对照溶液吡啶峰面积RSD为0.40%；影响因素试验，加速1个月试验注射用头孢他啶中吡啶含量均未超出含量限度（0.4%）；3种头孢他啶静脉注射溶液随时间的增加吡啶含量均有增加，避光下含量增加幅度略低于不避光，以生理盐水组增加幅度最小。结论通过试验建立了吡啶的HPLC标准工作曲线进行定量检测，其方法可靠，影响因素及加速试验可为该制剂包装贮存提供参考，3种稀释剂配置的注射液稳定性试验可为提高该药质量标准、临床合理配用、说明书的合理科学制定等提供参考。%Objective To study the detection method of pyridine in Ceftazidime for Injection to provide reference for in-creasing its quality standard,clinical dispensing use,rational package and storage,and revision of instruction. Methods The HPLC was adopted and the external standard used the pyridine content as the indicator ,the linear relationship test,precision test and stability test for the detection method were conducted;the 1-month accelerated test and the affecting factors trial were con-ducted for comparing the quality of products under this condition;the sample solution prepared by adopting the methods in the product manual was performed the stability test for comparing the content change of pyridine in different prepared solutions. Re-sults The linear regression equation for pyridine was Y=168 580X-2 451,R2=0.999 8,there was a good linear relationship with peak area within the range of 0.055 2~0.661 9μg;the precision test showed that RSD of pyridine chromatographic peak area was 0.29%;in the stability test,pyridine peak area RSD of the old and new pyridine control solution was 0.40%;in the influence factor tests,the 1-month accelerated tests showed that the pyridine content did not exceed the content limits (0.4%);in three kinds of ceftazidime intravenous solution ,the pyridine content was increased with time ,the content increased range in avoiding light was slightly lower than that without avoiding light ,which in the physiological saline group had smallest increase. Conclusion The established HPLC standard curve of pyridine by tests can be used for the quantitative detection of pyridine;the method is reliable, the influencing factors and accelerated test can provide a reference for the packaging and storage of this preparation;the stability test of injection solution prepared by three kinds of diluents can provide reference for improvement of drug standards and quality control,reasonable clinical use and making reasonable scientific product manual and so on.