scholarly journals A Validated Reverse Phase HPLC Analytical Method for Quantitation of Glycoalkaloids inSolanum lycocarpumand Its Extracts

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Renata Fabiane Jorge Tiossi ◽  
Mariza Abreu Miranda ◽  
João Paulo Barreto de Sousa ◽  
Fabíola Silva Garcia Praça ◽  
Maria Vitória Lopes Badra Bentley ◽  
...  

Solanum lycocarpum(Solanaceae) is native to the Brazilian Cerrado. Fruits of this species contain the glycoalkaloids solasonine (SN) and solamargine (SM), which display antiparasitic and anticancer properties. A method has been developed for the extraction and HPLC-UV analysis of the SN and SM in different parts ofS. lycocarpum, mainly comprising ripe and unripe fruits, leaf, and stem. This analytical method was validated and gave good detection response with linearity over a dynamic range of 0.77–1000.00 μg mL−1and recovery in the range of 80.92–91.71%, allowing a reliable quantitation of the target compounds. Unripe fruits displayed higher concentrations of glycoalkaloids (1.04% ± 0.01 of SN and 0.69% ± 0.00 of SM) than the ripe fruits (0.83% ± 0.02 of SN and 0.60% ± 0.01 of SM). Quantitation of glycoalkaloids in the alkaloidic extract gave 45.09% ± 1.14 of SN and 44.37% ± 0.60 of SM, respectively.

2020 ◽  
Vol 2020 ◽  
pp. 1-7
Author(s):  
Murad Abualhasan ◽  
Nihaya Wasif Odeh ◽  
Ghadeer Naser Younis ◽  
Oyoun Fadel Zeidan

Background. Sodium valproate has anticonvulsant activity and is structurally different to conventional antiepileptic drugs. The problem with valproic acid is the lack of a chromophore, which means that gas chromatography is the sole assay methodology. The introduction of benzoyl and phenyl groups to the molecule is a useful derivatisation, which enables the creation of detectable chromophores for HPLC analysis for pharmaceutical dosages as well as biological systems. Methodology. Sodium valproate was derivatised by the addition of a chromophore to its structure by introducing a methyl benzoyl or a phenyl group. Trichlorophenol and 2-hydroxyacetophenone were used to introduce phenyl and benzoyl groups to valproic acid, respectively. The reaction used was estrification reaction using coupling agents. An analytical method was then developed and validated using reverse-phase HPLC. The method was validated for parameters like linearity, range, accuracy precision, and robustness. Results. The developed method was easy and feasible and can be applied to both routine analysis and bioanalysis. The method was very sensitive and could quantify valproic acid at a very low concentration of 0.75 × 10−5 mg/ml. The developed method was found to be linear (R2 = 0.997), accurate, precise, and robust. Conclusion. The proposed chemical derivatisation and the developed analytical method are novel. The developed analytical procedure is the first of its kind; it is easy and feasible and can be used to quantify and detect sodium valproate at very low concentrations compared to other available methods in the literature.


Pharmaciana ◽  
2017 ◽  
Vol 7 (2) ◽  
pp. 169
Author(s):  
Florentinus Dika Octa Riswanto ◽  
Dita Maria Virginia ◽  
Dina Christin Ayuning Putri ◽  
Sri Hartati Yuliani

2021 ◽  
Vol 4 (1) ◽  
Author(s):  
Rod Chalk ◽  
William E. P. Greenland ◽  
Tiago Moreira ◽  
Jesse Coker ◽  
Shubhashish M. M. Mukhopadhyay ◽  
...  

AbstractWe describe an analytical method for the identification, mapping and relative quantitation of glycopeptides from SARS-CoV-2 Spike protein. The method may be executed using a LC-TOF mass spectrometer, requires no specialized knowledge of glycan analysis and exploits the differential resolving power of reverse phase HPLC. While this separation technique resolves peptides with high efficiency, glycans are resolved poorly, if at all. Consequently, glycopeptides consisting of the same peptide bearing different glycan structures will all possess very similar retention times and co-elute. Rather than a disadvantage, we show that shared retention time can be used to map multiple glycan species to the same peptide and location. In combination with MSMS and pseudo MS3, we have constructed a detailed mass-retention time database for Spike glycopeptides. This database allows any accurate mass LC-MS laboratory to reliably identify and quantify Spike glycopeptides from a single overnight elastase digest in less than 90 minutes.


2009 ◽  
Vol 20 (1) ◽  
pp. 24-32 ◽  
Author(s):  
João Paulo B. de Sousa ◽  
Ademar A. da Silva Filho ◽  
Paula C. P. Bueno ◽  
Luiz E. Gregório ◽  
Niege A. J. C. Furtado ◽  
...  

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