Two novel UPLC methods utilizing two different analytical columns and different detection approaches for the simultaneous analysis of velpatasvir and sofosbuvir: application to their co-formulated tablet

Abstract

In the present study two different RSLC columns, Acclaim RSLC 120 C18, 5.0 µm, 4.6 × 150 mm (column A) and Acclaim RSLC 120 C18, 2.2 µm, 2.1 × 100 mm (Column B) were utilized for the analysis of velpatasvir (VPS) in presence of sofosbuvir (SFV), where due to the encountered fluorescent properties of VPS fluorescent detection at 405 nm after excitation at 340 nm (Method 1) was used for its detection where the non-fluorescent SFV did not interfere. The same columns were further utilized for the simultaneous determination of SFV and VPS either in bulk form or in their combined tablet, where UV- spectrophotometric detection at 260 nm was selected for the simultaneous analysis of both drugs (Method 2). A mobile phase consisting of NaH2PO4, pH 2.5 (with phosphoric acid) and acetonitrile in a ratio of 60:40 v/v was used for both methods. The mobile phase was pumped at a flow rate of 1.0 mL/min when using column, A and 0.5 mL/min when using column B. The methods showed good linearity over the concentration ranges of 1.0–5.0 and 2.5–10.0 ng/mL for VPS when utilizing Method 1 A and B respectively. Where the linearity concentration range was from 30.0–150.0 to 120–600.0 ng/mL for VPS and SFV respectively when applying Method 2. Both methods 1 and 2 were performed by utilizing the two analytical columns. The different chromatographic parameters as retention time, resolution, number of theoretical plates (N), capacity factor, tailing factor and selectivity were carefully optimized. The results show that comparing the performance of the two utilized columns revealed that shorter column (2.1 mm × 100 mm) with small particle packing was superior to the longer column (4.6 × 150 mm) for the analysis of the studied drugs allowing a reduction of the analysis time by 70% without any detrimental effect on performance. This prompts the decrease of the investigation costs by saving money on organic solvents and expanding the overall number of analyses per day.

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“…The drug is available in the form of 100 mg tablets. The IUPAC name of VEL is Methyl { The literature survey revealed that the methods reported [5][6][7] for the estimation of SOF and VEL individually or in their combined dosage forms by UV Spectroscopy [8][9][10] and RP-HPLC method [11][12][13][14] . The proposed method is highly recommended in routine analysis where method is more economical, rapid, precise, and accurate.…”

Forced Degradation Studies and Development and Validation of HPLC-UV Method for the Analysis of Velpatasvir Copovidone Solid Dispersion

“…The official pharmacopeial monograph is also not available for the analysis of drug substance and pharmaceutical formulations. Very few analytical methods, focusing on simultaneous analysis of VEL and Sofosbuvir combined formulation, are reported in literature [ 13 , 14 , 15 , 16 , 17 , 18 ] Stability indicating methods for the analysis of VEL pure drug substance and degradation studies are also reported [ 19 , 20 , 21 , 22 , 23 ] but have limited information and discrepancies with published literature of FDA and MHRA [ 24 , 25 ]. As per MHRA public assessment report, VEL is photolabile, however it is reported stable in forced degradation studies published on UPLC [ 26 ].…”

Sensitive Determination of SARS-COV-2 and the Anti-hepatitis C Virus Agent Velpatasvir Enabled by Novel Metal–Organic Frameworks

“…To this end, VLP determination in the presence of sofosbuvir was reported using a plethora of methods, including LC–MS/MS, , UPLC-ESCI MS/MS, HPLC–MS/MS, and HPTLC, in biological fluids and clinical studies. In addition, the determination of the two drugs in their pharmaceutical formula was addressed utilizing UPLC, spectrofluorimetry, UPLC/spectrofluorimetry, and spectrophotometry . However, the determination range is somewhat expensive and time-consuming.…”