Abstract
Herein, a green liquid phase microextraction protocol using phthalic acid as switchable hydrophilicity solvent (SHS) is reported for the quantification of sildenafil in authentic human urine. The analyte was extracted onto phthalic acid solid particles which were produced through acidification of the sample. Its solidification was accomplished at ambient conditions without sample cooling. The determination of the sildenafil was carried out using high performance liquid chromatography-ultraviolet detection (HPLC-UV). The microextraction parameters that affect the extraction efficiency of the drug (i.e. SHS type and its concentration, acid type and concentration, extraction time, filter type) have been studied. The optimized analytical protocol involved the mixing of 300 μL of phthalate solution (0.75 M) with 600 μL of sample, followed by the addition of 50 μL of concentrated H3PO4. The produced solid was collected using membrane syringe filter (0.45 μm) and was finally dissolved in 500 μL of CH3OH. Method validation data showed determination coefficient ≥ 0.99 for the linear range of 50 – 2000 ng/mL. The limit of detection (LOD) and the lower limit of quantitation (LLOQ) were 30 and 100 ng/mL, respectively. The accuracy (expressed as % recovery) of the method ranged between 88.0 – 108.9 % while the precision (expressed as % RSD) was less than 17.8 % in all cases. The robustness of the microextraction procedure and the instrumental method were investigated using Plackett-Burman experimental designs. The applicability of the method was demonstrated by analyzing both spiked and authentic human urine samples after oral administration of drug-containing pharmaceutical formulation. The developed protocol offers cost-efficiency, handling simplicity, and high throughput. Its green character was evaluated using Green Analytical Procedure Index and Blue Applicability Grade Index.
Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Schedule a callDisclaimer: All third-party content on this website/platform is and will remain the property of their respective owners and is provided on "as is" basis without any warranties, express or implied. Use of third-party content does not indicate any affiliation, sponsorship with or endorsement by them. Any references to third-party content is to identify the corresponding services and shall be considered fair use under The CopyrightLaw.
