19F-核磁共振定量(19F-qNMR)法對添加入當歸苦參丸中的環(huán)丙沙星進行檢測,以4,4’-二氟二苯甲酮為內標,以氘代DMSO為溶劑,采集δ-120.3處環(huán)丙沙星信號和δ-104.8處內標信號面積,計算環(huán)丙沙星的含量。結果 以環(huán)丙沙星和內標信號面積比為縱坐標,環(huán)丙沙星和內標質量比為橫坐標,得到線性回歸方程為:Y=3.384 1X+0.114 8,R2=0.992,環(huán)丙沙星在5~30 mmol/L具有良好的線性,檢出限為7.798×10-2 mg/mL,定量限為0.260 mg/mL。建立的19F-qNMR法精密度、重復性、穩(wěn)定性、加樣回收率均符合檢測要求。結論 所建立的19F-qNMR法樣品制備簡單,檢測時間短,靈敏度高,適合對丸劑中非法添加的環(huán)丙沙星進行含量測定。;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 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."/> 19F核磁共振定量技術;環(huán)丙沙星;非法添加;4,4’-二氟二苯甲酮;19F-quantitative NMR;ciprofloxacin;illegally added drugs;4,4'-difluorobenzophenone"/>

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首頁 > 過刊瀏覽>2020年第43卷第6期 >2020,43(6):1075-1078. DOI:10.7501/j.issn.1674-6376.2020.06.016
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丸劑中非法添加環(huán)丙沙星的快速檢測方法研究

A rapid detection method for illegal addition of ciprofloxacin in pills

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