Journal
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
Volume 931, Issue -, Pages 111-116Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2013.05.013
Keywords
Phosphodiesterase-5 inhibitors; Ionic liquid; Dispersive liquid-liquid microextraction; Back extraction; Human plasma; Sildenafil; Vardenafil; Aildenafil
Funding
- Nature Science Foundation of China [81173018, 21105033, 81072596]
- Doctoral Fund of Ministry of Education of China [20110142120029]
- Scientific Research Foundation for Returned Scholars
- Program for New Century Excellent Talents in University, Ministry of Education of China [NCET-12-0213]
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A novel method which involved dispersive liquid-liquid microextraction (DLLME)-back extraction based on ionic liquid (IL) was developed for the determination of three phosphodiesterase-5 (PDE-5) inhibitors, sildenafil (SD), vardenafil (VD) and aildenafil (AD), in human plasma. DLLME based on IL as the extractant solvent and methanol as the dispersive solvent was the first step to extract PDE-5 inhibitors from sample solution; the other step of back extraction was followed by transferring target analytes from the IL to acidified aqueous solution. This two-step extraction ensured the compatibility of the final extractant phase, acidified aqueous solution herein, with the reversed phase high performance liquid chromatography-UV detection, and afforded clean extractant phase. The optimal extraction condition was obtained after systematical optimization. The sample solution (960 mu L) was extracted by 20 mu L of 1-octy1-3-methylimidazolium hexafluorophosphate in the presence of 20 mu L methanol and 300 mg mL(-1) NaCl with the assistance of vortex; IL phase enriched with the target analytes was then extracted by 10% acetic acid aqueous solution. Good linearity ranges (SD 1-500 ng mL(-1), VD 2-2000 ng mL(-1) and AD 2-2000 ng mL(-1)) with suitable r(2) (=0.9999) were achieved. Limits of detection (LODs) in pure water were 0.15 ng mL(-1), 0.30 ng mL(-1) and 0.43 ng mL(-1) for VD, SD and AD, respectively. Intra-day and inter-day relative standard deviations were below 6.38%. Finally, this method was applied for the determination of PDE-5 inhibitors in human plasma with satisfactory LODs of 0.92 ng mL(-1), 1.19 ng mL(-1) and 2.69 ng mL(-1) for VD, SD and AD, respectively. Acceptable absolute recoveries were obtained from 100.4% to 103.9%. The developed method afforded a convenient, fast and cost-saving operation with high extraction efficiency for the test analytes. It has potential to be applicable to biological samples. (C) 2013 Elsevier B.V. All rights reserved.
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