High performance thin-layer and high performance liquid chromatography coupled with photodiode array and fluorescence detectors for analysis of valsartan and sacubitril in their supramolecular complex with quantitation of sacubitril-related substance in raw material and tablets. (28th March 2018)

• Record Type: Journal Article
• Authors: Ragab, Marwa A A; Galal, Shereen M; Korany, Mohamed A; Ahmed, Aya R
• Is Part Of: Journal of chromatographic science. Volume 56:Number 6(2018:Jul.)
• Page Start: 498
• Page End: 509
• Publication Date: 2018-03-28
• Subjects: Chromatographic analysis -- Periodicals; 543.8
• DOI: 10.1093/chromsci/bmy021
• Languages: English
• ISSNs: 0021-9665

Abstract

Abstract: Valsartan (VAL) and sacubitril (SAC) are combined in a supramolecular complex, LCZ696, which is a newly approved remedy for heart failure. SAC-related substance (biphenyl methyl pyrrolidinone [BMP]) which also appears as an intermediate during SAC synthesis is considered to be a suspected impurity for SAC and/or LCZ696 tablets. The study investigates the analysis of VAL and SAC in their supramolecular complex along with SAC-related substance, BMP, using high performance thin-layer chromatography (HPTLC) and high performance liquid chromatography (HPLC) with two different detectors; fluorescence detector (FLD) and diode array detector (DAD). The work aimed at analyzing BMP at low levels in the presence of its parent drug, SAC. BMP was successfully analyzed at a level of 0.167, 1 and 3% of its parent drug, SAC upon using HPLC-FLD, HPLC-DAD and HPTLC, respectively. For HPLC-FLD, the detector was set at λ ex/ λ em (nm/nm): 0–4.5 min at 255/374; 4.5–6 min at 255/314, for achieving an adequate sensitivity of the method to monitor and quantify VAL and SAC in the presence of BMP. Low limits of detection (8.3, 3.3 and 1.7 ng mL −1 ) and limits of quantitation (25, 10 and 5 ng mL −1 ) values obtained for VAL, SAC and BMP, respectively, upon using FLD suggest that low level of baseline noise enables the detection and quantitation of low BMP concentration.