Related Experiment Video
Updated: Jul 30, 2026
Accessing Valuable Ligand Supports for Transition Metals: A Modified, Intermediate Scale Preparation of 1,2,3,4,5-Pentamethylcyclopentadiene
Published on: March 20, 2017
Concurrent quantification of novel cyclometalated iridium-based photosensitizer and 5-fluorouracil using RP-HPLC:
Pragati Ramesh Kumbhar1, Vaibhavi Meghraj Desai1, Sumit Punia2
1Industrial Research Laboratory, Department of Pharmacy, Birla Institute of Technology and Science, Pilani (BITS-PILANI), Pilani Campus, Vidya Vihar, Pilani, Rajasthan 333031, India.
Background:
Combination therapies for skin cancer are emerging as effective strategies to overcome limitations of monotherapies, such as limited efficacy, resistance development, and recurrence. Chemo-photodynamic therapy represents a promising approach for this. In this study, novel cyclometalated iridium-based photosensitizer was investigated in combination with 5-fluorouracil. As the photosensitizer is novel, no analytical method has been reported for its simultaneous estimation with 5-FU. Such a method is essential for quantifying both analytes in nanoformulations, enabling pharmacokinetic and skin permeation studies critical for development of chemo-photodynamic therapy.
Method:
A simultaneous RP-HPLC method was developed using a C18-column with an isocratic mobile phase of acetonitrile and pH 4.0 buffer (80:20v/v) at a flow rate of 1.0 mL/min. Detection was performed at 265 nm. The method was validated in accordance with ICH guidelines, including forced-degradation studies, and applicability was evaluated using nanodispersion and skin permeation samples.
Results:
Good resolution was achieved between CIBP and 5-FU, with retention times of 5.944 and 2.714 min, respectively. The method showed excellent linearity (r2>0.999) at concentration range of 500-12,000 ng/mL. High accuracy was observed, with recoveries of 100.74-101.35% for CIBP and 100.94-101.05% for 5-FU. High sensitivity was demonstrated, with LOD/LOQ values of 6.89/20.90 ng/mL for CIBP and 5.62/17.04 ng/mL for 5-FU. Precision studies showed %RSD < 2% for both analytes.
Conclusion:
The validated method is reliable, economical, and suitable for routine quantification of both analytes in stability studies, drug-encapsulation, in-vitro release, and ex-vivo skin permeation samples, supporting quality control and dermatokinetics profiling of dual-drug-loaded nanodispersion.
Insights
A new HPLC method quantifies a novel iridium photosensitizer and 5-fluorouracil for skin cancer therapy. This reliable method supports quality control and development of combination chemo-photodynamic treatments.
Area of Science:
- Analytical Chemistry
- Pharmaceutical Sciences
- Dermatology
Background:
- Combination therapies, including chemo-photodynamic therapy, offer improved efficacy for skin cancer over monotherapies.
- Novel iridium-based photosensitizers are being explored for chemo-photodynamic therapy, necessitating analytical methods for their evaluation.
- A simultaneous analytical method is crucial for quantifying novel photosensitizers and chemotherapeutics like 5-fluorouracil (5-FU) in nanoformulations.
Purpose of the Study:
- To develop and validate a simultaneous RP-HPLC method for quantifying a novel cyclometalated iridium-based photosensitizer (CIBP) and 5-fluorouracil (5-FU).
- To enable pharmacokinetic/pharmacodynamic and skin permeation studies for chemo-photodynamic therapy development.
- To support quality control and dermatokinetics profiling of dual-drug-loaded nanodispersion.
Main Methods:
- Development of a simultaneous reversed-phase high-performance liquid chromatography (RP-HPLC) method using a C18 column.
- Isocratic elution with an acetonitrile and pH 4.0 buffer mobile phase (80:20 v/v) at a flow rate of 1.0 mL/min.
- Detection at 265 nm and validation according to ICH guidelines, including forced-degradation and applicability studies.
Main Results:
- Achieved good chromatographic resolution (>3) between CIBP and 5-FU with distinct retention times.
- Demonstrated excellent linearity (r² > 0.999) over a wide concentration range (500-12,000 ng/mL).
- Exhibited high accuracy (recoveries 100.74-101.35% for CIBP, 100.94-101.05% for 5-FU) and sensitivity (LOD/LOQ in ng/mL range).
- Confirmed high precision with %RSD < 2% for both analytes.
Conclusions:
- The validated RP-HPLC method is reliable, economical, and suitable for routine quantification of CIBP and 5-FU.
- The method supports stability studies, drug encapsulation, in-vitro release, and ex-vivo skin permeation analyses.
- This analytical tool is essential for advancing the development of chemo-photodynamic therapy for skin cancer.
More Related Videos
08:57Sample Extraction and Simultaneous Chromatographic Quantitation of Doxorubicin and Mitomycin C Following Drug Combination Delivery in Nanoparticles to Tumor-bearing Mice
Published on: October 5, 2017
09:33Determination of the Photoisomerization Quantum Yield of a Hydrazone Photoswitch
Published on: February 7, 2022
