[关键词]
[摘要]
目的 建立一种丸剂中非法添加环丙沙星的快速检测方法。方法 通过19F-核磁共振定量(19F-qNMR)法对添加入当归苦参丸中的环丙沙星进行检测,以4,4’-二氟二苯甲酮为内标,以氘代DMSO为溶剂,采集δ-120.3处环丙沙星信号和δ-104.8处内标信号面积,计算环丙沙星的含量。结果 以环丙沙星和内标信号面积比为纵坐标,环丙沙星和内标质量比为横坐标,得到线性回归方程为:Y=3.384 1X+0.114 8,R2=0.992,环丙沙星在5~30 mmol/L具有良好的线性,检出限为7.798×10-2 mg/mL,定量限为0.260 mg/mL。建立的19F-qNMR法精密度、重复性、稳定性、加样回收率均符合检测要求。结论 所建立的19F-qNMR法样品制备简单,检测时间短,灵敏度高,适合对丸剂中非法添加的环丙沙星进行含量测定。
[Key word]
[Abstract]
Objective To establish a rapid detection method for illegal addition of ciprofloxacin in pills. Methods The qualitative examination of the presence of illegally added ciprofloxacin in the pill was conducted by the 19F-quantitative nuclear magnetic resonance (19F-qNMR) method. 4, 4'-difluorobenzophenone as an internal standard and DMSO-d6 as the solvent were used in 19F-qNMR. The ciprofloxacin content was calculated by comparing the response signal (δ -120.3) of sample and internal standard (δ-104.8). Results Taking the area ratio of ciprofloxacin and internal standard signal as ordinate and the mass ratio of ciprofloxacin and internal standard as abscissa, the linear regression equation was:Y=3.384 1X + 0.114 8, R2>0.99. This method had a good linearity in the range of 5-30 mmol/L. The detection limit was 7.798×10-2 mg/mL and the limit of quantitation was 0.260 mg/mL. The precision, repeatability, stability and recovery rate of 19F-qNMR method meet the requirements of detection. The mass fraction of ciprofloxacin was 83.94%, RSD was 0.54%, and the results were accurate. Conclusion This method requires short detection time and simple sample preparation, has high sensitivity. 19F-qNMR is suitable for the content determination of ciprofloxacin illegally added in pills.
[中图分类号]
R927.2
[基金项目]
甘肃省科技重大专项(17ZD2FA009);广西自治区第五批特聘专家支持