色谱

色谱 ›› 2015, Vol. 33 ›› Issue (7): 765-770.DOI: 10.3724/SP.J.1123.2015.02063

• 研究论文 • 上一篇    下一篇

新型液相色谱?荧光检测法测定药物剂型和人血浆中的他达拉非和盐酸达泊西汀

MAHA Hegazy1, AMIRA Kessiba2, MOHAMED Abdelkawy1,3, AHMED EMAD El Gindy2   

  1. 1. Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Cairo 11562, Egypt;
    2. Pharmaceutical Chemistry Department, Faculty of Pharmacy, Misr International University, Cairo 41611, Egypt;
    3. Pharmaceutical Chemistry Department, Faculty of Pharmacy, Future University, New Cairo 11856, Egypt
  • 收稿日期:2015-02-10 出版日期:2015-07-08 发布日期:2015-07-27
  • 通讯作者: MAHA Hegazy

A novel liquid chromatographic method with fluorescence detection for quantitation of tadalafil and dapoxetine hydrochloride in pharmaceutical dosage form and human plasma

MAHA Hegazy1, AMIRA Kessiba2, MOHAMED Abdelkawy1,3, AHMED EMAD El Gindy2   

  1. 1. Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Cairo 11562, Egypt;
    2. Pharmaceutical Chemistry Department, Faculty of Pharmacy, Misr International University, Cairo 41611, Egypt;
    3. Pharmaceutical Chemistry Department, Faculty of Pharmacy, Future University, New Cairo 11856, Egypt
  • Received:2015-02-10 Online:2015-07-08 Published:2015-07-27

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摘要：

Tadalafil (TAD) and dapoxetine HCl (DAP) are recently co-formulated and both show native fluorescence. Therefore, a novel, accurate, specific and sensitive reversed-phase high performance liquid chromatographic method with fluorescence detection was developed and validated for their separation and quantitation in dosage form and human plasma using avanafil as an internal standard (IS). Separation was achieved using isocratic elution within 7.0 min on C18 column and acetonitrile-0.15% triethylamine (40 : 60, v/v; pH 4) as a mobile phase. The flow rate was 1.0 mL/min and the detection was time-programmed at 330, 410 and 370 nm for TAD, DAP and IS, respectively, after excitation at 236 nm. The linear ranges from 0.01 to 30.00 μg/mL for each drug with the limits of detection of 4.20 and 7.20 ng/mL for TAD and DAP, respectively. The method was validated in accordance to the International Conference on Harmonization (ICH) guidelines and was successfully applied to spiked human plasma with mean recoveries of 98.17% and 98.83% for TAD and DAP respectively.

关键词: dapoxetine HCl (DAP), dosage form, fluorescence detection, high performance liquid chromatography (HPLC), human plasma, tadalafil (TAD)

Abstract:

Tadalafil (TAD) and dapoxetine HCl (DAP) are recently co-formulated and both show native fluorescence. Therefore, a novel, accurate, specific and sensitive reversed-phase high performance liquid chromatographic method with fluorescence detection was developed and validated for their separation and quantitation in dosage form and human plasma using avanafil as an internal standard (IS). Separation was achieved using isocratic elution within 7.0 min on C18 column and acetonitrile-0.15% triethylamine (40 : 60, v/v; pH 4) as a mobile phase. The flow rate was 1.0 mL/min and the detection was time-programmed at 330, 410 and 370 nm for TAD, DAP and IS, respectively, after excitation at 236 nm. The linear ranges from 0.01 to 30.00 μg/mL for each drug with the limits of detection of 4.20 and 7.20 ng/mL for TAD and DAP, respectively. The method was validated in accordance to the International Conference on Harmonization (ICH) guidelines and was successfully applied to spiked human plasma with mean recoveries of 98.17% and 98.83% for TAD and DAP respectively.

Key words: dapoxetine HCl (DAP), dosage form, fluorescence detection, high performance liquid chromatography (HPLC), human plasma, tadalafil (TAD)

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