摘要
目的:建立帕司烟肼片中间氨基酚和游离肼的HPLC测定方法。方法:间氨基酚色谱柱:Agilent ZORBAX SB-Aq(4.6 mm×250 mm,5μm);流动相:甲醇-10%四丁基氢氧化铵溶液-0.05 mol·L^(-1)磷酸二氢钠(100∶2∶900);检测波长为220 nm;游离肼色谱柱:Diamonsil Plus C(4.6 mm×150 mm,5μm);流动相:0.1%乙二胺四乙酸二钠-乙腈(31∶69);检测波长为310 nm。结果:间氨基酚和游离肼的线性范围分别为0.1010~20.19μg·m L^(-1)和0.2590~51.80μg·m L^(-1)(r≥0.9999),检测限分别为0.1 ng、0.04 ng,平均回收率分别为99.39%、99.16%(RSD≤1.0%,n=8)。结论:该方法专属性好、操作简便、快速准确,可用于帕司烟肼片中间氨基酚和游离肼的的检测。
Objective:To establish an HPLC method for determination of 3-aminophenol and free hydrazine in Pasiniazid tablets.Methods:3-Aminophenol The eluate obtained was analyzed by HPLC method with Agilent ZORBAX SB-Aq(250 mm×4.6 mm,5μm),using methanol-10%Tetrabutylammonium hydroxide-0.05 mol·LNa HPObuffer(100∶2∶900)as mobile phase,and the detection wavelength was set at 220 nm.Free hydrazine The eluate obtained was analyzed by HPLC method with Diamonsil Plus C_(18)(150 mm×4.6 mm,5μm),using 0.1%EDTA-acetonitrilr(30∶70)as mobile phase,and the detection wavelength was set at 310 nm.Results:3-aminophenol and free hydrazine showed good linearity in the ranges of 0.1010-20.19μg·mL^(-1),0.2590-51.80μg·mL^(-1)(r≥0.9999)respectively.The detection limit were 0.1 ng、0.04 ng respectively.The average recovery values values of 3-aminophenol and free hydrazine of were99.39%、99.16%(RSD≤1.0%,n=8)respectively.Conclusion:The method is simple with high accuracy and reproducible,which can be used for the determination of 3-aminophenol and free hydrazine in Pasiniazid tablets.
作者
刘志辉
LIU Zhi-hui(The Food and Drug Control of Meizhou Institute,Guangdong Meizhou 514071,China)
出处
《中国药物评价》
2022年第5期395-398,共4页
Chinese Journal of Drug Evaluation
关键词
帕司烟肼片
间氨基酚
游离肼
高效液相色谱(HPLC)
Pasiniazid tablets
3-aminophenol
Free hydrazine
High performance liquid chromatography(HPLC)
