Optimization of Mobile Phase Conditions for TLC Methods Used in Pharmaceutical Analyses

Costanzo, Samuel J.

doi:10.1093/chromsci/35.4.156

Cited by 6 publications

(2 citation statements)

References 6 publications

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“…Different molecules partition differently between the free and absorbed state that is the equilibria between these two states is not the same. [ 12 ]…”

Section: Resultsmentioning

confidence: 99%

Isolation and structure determination of 24-methylenecycloartanyl ferulate from Indian rice bran and its quantitative analysis

2016

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Background:γ-oryzanol is a major bioactive constituent in rice. Most of the literature reports isolation of 24-methylenecycloartanyl ferulate (24-mCAF) from rice bran oil (RBO) of other than Indian variety. Current research has successfully applied high-performance thin layer chromatography (HPTLC) method for isolation of 24-mCAF from Indian variety (Indrayani) of RBO.Materials and Methods:HPTLC method was developed for standard γ-oryzanol using tinidazole as an internal standard. The proposed HPTLC method was optimized and validated as per the guidelines stated by the International Conference on Harmonization Q2 R1 recommendations. The mobile phase composed of toluene:ethyl acetate:methanol (15.0:1.7:3.3, (v/v/v) was selected because well-resolved peaks were obtained. The optimum wavelength chosen for detection and quantitation was 317 nm.Results:The retention factors for tinidazole, 24-mCAF, and CAF were found to be 0.27 ± 0.02, 0.72 ± 0.02, and 0.79 ± 0.02, respectively. The percent content of 24-mCAF in ethanol fraction was found to be 1.02%. The 24-mCAF was isolated from RBO using HPTLC method.Conclusion:The characterization data of 1D, 2D spectral analysis confirm that the isolated compound 1 is 24-mCAF.SUMMARY HPTLC method was developed for standard γ-oryzanol using tinidazole as an internal standardThe proposed HPTLC method was optimized and validated as per the guidelines stated by the ICH Q2 R1 recommendationsThe characterization data of 1D, 2D spectral analysis confirms that the isolated compound is 24-methylenecycloartanyl ferulateIn this work, high purity 24-mCAF was successfully isolated from crude RBO using HPTLC with a solvent system composed toluene: ethyl acetate: methanol (15.0:1.7:3.3, v/v/v) Abbreviations used: RBO: Rice Bran Oil, CAF: Cycloartenol ferulic acid, 24-mCAF: 24-Methylcycloartenol ferulic acid, HPLC: High-Performance Liquid Chromatography, HPTLC: High-Performance Thin Layer Chromatography, 1H: Proton nuclear magnetic resonance spectroscopy, 13C: Carbon-13 nuclear magnetic resonance spectroscopy, COSY: Correlation spectroscopy, NOESY: Nuclear overhauser effect spectroscopy, HMBC: Heteronuclear multiple bond correlation nuclear magnetic resonance spectroscopy, HSQC: heteronuclear single quantum coherence nuclear magnetic resonance spectroscopy.

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“…Different molecules partition differently between the free and absorbed state that is the equilibria between these two states is not the same. [ 12 ]…”

Section: Resultsmentioning

confidence: 99%

Isolation and structure determination of 24-methylenecycloartanyl ferulate from Indian rice bran and its quantitative analysis

2016

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“…It is also sometimes difficult to find suitable solid components and developing systems for these experiments, especially when separating isomeric mixtures. 9,10 Nuclear magnetic resonance (NMR) spectroscopy is a crucial analytical technique for natural product research because it provides tremendous structural information. Recently, it has become a reliable tool for quantitative studies.…”

Section: Introductionmentioning

confidence: 99%

Compositional variation of atranorin‐related components of lichen Myelochroa leucotyliza dependent on extraction solvent and their quantitative analysis by qHNMR

Ojha

Kil

Youn

et al. 2021

Phytochemical Analysis

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Introduction: Quantitative nuclear magnetic resonance (qNMR) is one of the effective and reliable quantification tools for natural product research. Myelochroa leucotyliza belongs to the genus Myelochroa, a common foliose lichen genus found in the Korean Peninsula, and has not been quantitatively analysed using NMR. Previous chemical studies on M. leucotyliza have been limited to the main components by traditional thin-layer chromatography (TLC) experiments.Objective: We explored the stability of atranorin, a major component of M. leucotyliza, in methanol and acetone using NMR and characterised the changes in the chemical profiles of the lichen extracts in methanol and acetone using qNMR.Methodology: Atranorin transformation in the presence of methanol was analysed using time-dependent proton ( 1 H)-NMR analysis (600 MHz NMR spectrometer). A 1 H qNMR (qHNMR) method was established using dimethyl sulfone as the internal standard for quantifying the selected components isolated from M. leucotyliza.Homogenous mixtures of the samples were dissolved in deuterated chloroform.Results: Time-dependent 1 H-NMR experiments revealed that atranorin (5) from lichen M. leucotyliza decomposed into atraric acid (1) and methyl haemmatommate (2) in methanol. Four components were identified from M. leucotyliza: 1, 2, usnic acid (4), and 5, and their respective contents were determined using qHNMR. The percentages (w/w) of 1, 2, and 4 in the methanol extract were calculated as 5.66%, 0.69%, and 0.90%, while those of 1, 4, and 5 in the acetone extract were 1.70%, 1.68%, and 19.11%, respectively. Conclusion:We used qHNMR to effectively analyse quantitative compositional variations in two different M. leucotyliza extracts and reliably determined the chemical conversion of the unstable compound atranorin.

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Thin-Layer Chromatography

Poole

2003

The Essence of Chromatography

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Optimization of Mobile Phase Conditions for TLC Methods Used in Pharmaceutical Analyses

Cited by 6 publications

References 6 publications

Isolation and structure determination of 24-methylenecycloartanyl ferulate from Indian rice bran and its quantitative analysis

Isolation and structure determination of 24-methylenecycloartanyl ferulate from Indian rice bran and its quantitative analysis

Compositional variation of atranorin‐related components of lichen Myelochroa leucotyliza dependent on extraction solvent and their quantitative analysis by qHNMR

Thin-Layer Chromatography

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