丸剂中非法添加环丙沙星的快速检测方法研究  

A rapid detection method for illegal addition of ciprofloxacin in pills

作　　者：白洁[1,2] 刘阳 刘静[3] 袁松[3] 张涛[4] 朱雪妍 杨平荣 BAI Jie;LIU Yang;LIU Jing;YUAN Song;ZHANG Tao;ZHU Xueyan;YANG Pingrong(Lan Zhou University,Lanzhou 730000,China;Gansu Institute for Drug Control,Lanzhou 730000,China;National Institutes for Food and Drug Control,Beijing 102629,China;Guangxi Institute for Food and Drug Control,Nanning 530021,China)

机构地区：[1]兰州大学,甘肃兰州730000 [2]甘肃省药品检验研究院,甘肃兰州730000 [3]中国食品药品检定研究院,北京102629 [4]广西壮族自治区食品药品检验所,广西南宁530021

出　　处：《药物评价研究》2020年第6期1075-1078,共4页Drug Evaluation Research

基　　金：甘肃省科技重大专项(17ZD2FA009);广西自治区第五批特聘专家支持。

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=3.3841X+0.1148,R2=0.992,环丙沙星在5~30 mmol/L具有良好的线性,检出限为7.798×10-2mg/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。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 19FqNMR.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=3.3841X+0.1148,R2>0.99.This method had a good linearity in the range of 5—30 mmol/L.The detection limit was 7.798×10-2mg/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.

关 键 词：19F核磁共振定量技术 环丙沙星 非法添加 4 4’-二氟二苯甲酮 

分 类 号：R927.2[医药卫生—药学]