Validated stability-indicating GC-MS method for characterization of forced degradation products of trans-caffeic acid and trans-ferulic acid

Islamčević Razboršek, Maša (author), Ivanović, Milena (author), Kolar, Mitja (author)

When dealing with simple phenols such as caffeic acid (CA) and ferulic acid (FA), found in a variety of plants, it is very important to have control over the most important factors that accelerate their degradation reactions. This is the first report in which the stabilities of these two compounds have been systematically tested by exposure to various different factors. Forced degradation studies were performed on pure standards (trans-CA and trans-FA), dissolved in different solvents and exposed to different oxidative, photolytic and thermal stress conditions. Additionally, a rapid, sensitive, and selective stability-indicating gas chromatographic-mass spectrometric method was developed and validated for determination of trans-CA and trans-FA in the presence of their degradation products. Cis-CA and cis-FA were confirmed as the only degradation products in all the experiments performed. All the compounds were perfectly separated by gas chromatography (GC) and identified using mass spectrometry (MS), a method that additionally elucidated their structures. In general, more protic solvents, higher temperatures, UV radiation and longer storage times led to more significant degradation (isomerization) of both trans-isomers. The most progressive isomerization of both compounds (up to 43%) was observed when the polar solutions were exposed to daylight at room temperature for 1 month. The method was validated for linearity, precision as repeatability, limit of detection (LOD) and limit of quantitation (LOQ). The method was confirmed as linear over tested concentration ranges from 1−100 mg L$^{−1}$ (r$^2$s were above 0.999). The LOD and LOQ for trans-FA were 0.15 mg L$^{−1}$ and 0.50 mg L$^{−1}$, respectively. The LOD and LOQ for trans-CA were 0.23 mg L$^{−1}$ and 0.77 mg L$^{−1}$, respectively.

• Language: English
• Keywords: caffeic acid, ferulic acid, stability studies, GC-MS, forced degradation
• Work type: Article
• Typology: 1.01 - Original Scientific Article
• Organization: FKKT - Faculty of Chemistry and Chemical Technology
• Publication status: Published
• Publication version: Version of Record
• Year: 2021
• Number of pages: 12 str.
• Numbering: Vol. 26, iss. 9, art. 2475
• PID: 20.500.12556/RUL-135298
• UDC: 66
• ISSN on article: 1420-3049
• DOI: 10.3390/molecules26092475
• COBISS.SI-ID: 61605891
• Publication date in RUL: 07.03.2022

Record is a part of a journal

• Title: Molecules
• Shortened title: Molecules
• Publisher: MDPI
• ISSN: 1420-3049
• COBISS.SI-ID: 18462981

Licences

• License: CC BY 4.0, Creative Commons Attribution 4.0 International
• Link: http://creativecommons.org/licenses/by/4.0/
• Description: This is the standard Creative Commons license that gives others maximum freedom to do what they want with the work as long as they credit the author.
• Licensing start date: 01.05.2021

Secondary language

• Language: Slovenian
• Keywords: kofeinska kislina, prisilna degradacija, študija stabilnosti

Projects

• Funder: ARRS - Slovenian Research Agency
• Project number: P2-0006
• Name: Fizikalno kemijski pojavi na površinskih plasteh in uporaba nanodelcev

• Funder: ARRS - Slovenian Research Agency
• Project number: P1-0153
• Name: Raziskave in razvoj analiznih metod in postopkov