反相高效液相色谱法和气相色谱法测定盐酸芬氟拉明片含量的比较研究

Comparative Study on Determination of Fenfluramine Hydrochloride Tablets by RP-HPLC and GC

目的 :研究一种用反相高效液相色谱测定盐酸芬氟拉明 (FH)片含量的方法 ,并与法定气相色谱法作比较研究。方法 :以水为溶剂处理样品 ,采用AlltimaC18柱为色谱柱 ,以 0 0 5mol·L-1磷酸液 (用三乙胺调 pH2 5 ) -甲醇 (5 0∶5 0 )为流动相 ,紫外检测波长 2 5 4nm ,流速 1 0mL·min-1,柱温 30℃。结果 :FH浓度在0 2 0～ 1 0mg·mL-1浓度范围内呈良好线性关系 (r =0 9999) ,最低检测浓度为 2 5 μg·mL-1,日内、日间精密度 (RSD)分别为 0 9% (n =4)和 0 7% (n =6 ) ,平均回收率为 99 4% ,RSD =1 0 % (n =5 )。结论 :高效液相色谱法采用水作溶剂 ,辅料不干扰测定 ,所得结果与理论值一致 ;而气相色谱法采用氯仿作溶剂 ,不同的处方其辅料对FH的溶出有干扰 ,可能导致测定结果偏低 ,应引起重视。

Objective:To establish an accurate method for determination of fenfluramine hydrochloride tablets by RP-HPLC ,and it was quantitatively studied in comparison with official GC method.Methods:the RP-HPLC method using Alltima C 18 column as analytical column,0 05 mol·L -1 phosphoric acid solution(adjusted pH to 2 5 with triethylamine)-methanol(50∶50)as the mobile phase.Detection wavelength was 254 nm.Flow rate was 1 0 mL·min -1 .Column temperature was 30℃.Results:There was a good linear within the range of 0 20～1 0 mg·mL -1 for fenfluramine hydrochloride with r=0 999 9. The average recovery was 99 4%( RSD =1 0%, n =5).The precision within-day RSD was 0 9%( n =4)and between-day RSD was 0 7%( n =6).The detection limit was less than 2 5 μg·mL -1 .Conclusion:Comparing with the GC method,the proposed RP-HPLC method has no interference in the assay by excipients and is more convenient,rapid,accurate and precise.