目的 建立一種丸劑中非法添加環(huán)丙沙星的快速檢測方法。方法 通過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(nèi)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(nèi)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(nèi)標信號面積比為縱坐標，環(huán)丙沙星和內(nèi)標質(zhì)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.

R927.2

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