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中国药物评价 ›› 2022, Vol. 39 ›› Issue (5): 395-398.

• 评价技术与方法 • 上一篇    下一篇

帕司烟肼片中间氨基酚和游离肼的检测

刘志辉   

  1. 梅州市食品药品监督检验所, 广东 梅州 514071
  • 收稿日期:2022-03-04 修回日期:2022-06-25 出版日期:2022-10-28 发布日期:2022-10-28

Determination of 3-aminophenol and Free Hydrazine in Pasiniazid Tablets

  1. The Food and Drug Control of Meizhou Institute,Guangdong Meizhou 514071,China
  • Received:2022-03-04 Revised:2022-06-25 Online:2022-10-28 Published:2022-10-28

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,5 μm);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 C18(4.6 mm×150 mm,5 μm);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0.101 0~20.19 μg·mL-1和0.259 0~51.80 μg·mL-1 (r≥0.999 9),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。

关键词: font-size:medium, ">帕司烟肼片;间氨基酚;游离肼;高效液相色谱(HPLC)

Abstract: 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·L-1 NaH2PO4 buffer(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 C18 (150 mm×4.6 mm,5 μm), 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 0.101 0-20.19 μg·mL-1, 0.259 0-51.80 μg·mL-1 (r≥0.999 9) respectively. The detection limit were 0.1 ng、0.04 ng respectively. The average recovery values values of 3-aminophenol and free hydrazine of were 99.39%、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.

Key words: font-size:medium, ">Pasiniazid tablets; 3-aminophenol; Free hydrazine; High performance liquid chromatography(HPLC)

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