TY - JOUR T1 - Development and validation of a novel HPLC-UV method for the determination of faradiol in creams including Marigold (Calendula officinalis L.) extract AU - Ceylan, Burhan PY - 2025 DA - July Y2 - 2024 DO - 10.12991/jrespharm.1734461 JF - Journal of Research in Pharmacy JO - J. Res. Pharm. PB - Marmara University WT - DergiPark SN - 2630-6344 SP - 1461 EP - 1467 VL - 29 IS - 4 LA - en AB - A straightforward, quick, and sensitive high-performance liquid chromatography (HPLC) technique was created to quantify the triterpene alcohol faradiol present in cosmetic creams that contain extract from marigold (Calendula officinalis L.). The mobile phase consisted of 95:5 methanol:water (2% o-phosphoric acid) with an isocratic elution and a flow rate of 1.3 mL/min. The stationary phase was a C18 (5 μm × 4.6 mm × 150 mm) column. Throughout the separation, a constant temperature of 35 ºC was maintained. Thirty μL was the injection volume. At 6.38±0.20 min, the faradiol peak was eluted. The International Conference on Harmanization (ICH) criteria for linearity, limit of detection, limit of quantitation, selectivity, sensitivity, robustness, accuracy, and precision were followed in the validation process. The limits of quantification and detection were 0.01 μg/mL and 0.003, in respective order. The arrangement of linear expression was between 0.01 and 30 μg/mL. For both the daily and hourly analysis, the relative standard deviation values were less than 1.20%. A variety of cosmetic goods were analysed using the suggested approach. The technique is anticipated to be appropriate for regular triterpene alcohol faradiol analysis, quality assurance, and standardisation of cosmetic cream products. KW - Faradiol KW - Margiold creams KW - HPLC-UV KW - Validation CR - [1] European Pharmacopoeia Supplement. German Edition, Stuttgart: Deutscher Apotheker Verlag, 1015. 1999. CR - [2] Zitterl-Eglseer K, Sosa S, Jurenitsch J, Schubert-Zsilavecz M, Della Loggia R, Tubaro A, Bertoldi M, Franz C. Antiodematous activities of the main triterpendiol esters of marigold (Calendula officinalis L.). J Ethnopharmacol. 1999; 57(2): 139-144. https://doi.org/10.1016/s0378-8741(97)00061-5 CR - [3] Blumenthal M. The complete German commission E monographs. Austin: American Botonical Council. 1998. CR - [4] Hansel R, Keller K, Rimpler H, Schneider G. Hagers bandbuch der pharmazeutischen praxis. Berlin, Springer, 1992. CR - [5] Isaac O. Die ringelblume-botanic, chemie, pharmakologie, toxikologie, pharmazie and therapeutische Verwendung. Stuttgart, 1992. CR - [6] Della Loggia, Tubaro A, Sosa S, Becher H, Saar S, Isaac O. The role of triterpenoids in the topical anti-inflammatory activity of Calendula officinalis L. flowers. Planta Medica. 1994; 60(6): 516-520. CR - [7] Doddrell DM, Khong PW, Lewis KG. The stereochemical dependence of 13C chemical shifts in olean-12-enes and urs-12-enes as an aid to structural assignment. Tetrahedron. 1974; 15(27): 2381-2384. https://doi.org/10.1016/S0040-4039(01)92261-0 CR - [8] Neukirch H, D’Ambrosio M, Sosa S, Altinier G, Della Loggia R, Guerriero A. Improved anti-inflammatory activity of three new terpenoids derived by systematic chemical modifications, from the abundant triterpenes of the flower plant Calendula officinalis L. Chem Biodivers. 2005; 2(5): 657-671. https://doi.org/10.1002/cbdv.200590042 CR - [9] Hamburger M, Agler S, Baumann D, Förg A, Weinreich B. Preparative purification of the major anti-inflammatory triterpenoids esters from marigold (Calendula officinalis L.). Fitoterapia. 2003; 74(4): 328-338. https://doi.org/10.1016/s0367-326x(03)00051-0 CR - [10] Zittler-Eglserr K, Reznicek G, Jurenitsch J, Novak J, Zittler W, Franz C. Morphogenetic variability of faradiol monoesters in marigold Calendula officinalis L. Phytochem Anal. 2001; 12(3): 199-201. https://doi.org/10.1002/pca.582 CR - [11] Nicolus C, Sievers-Engler A, Murillo R, D’Ambrosio M, Lammerhofer M, Merfort I. Mastering analytical challenges for the characterization of pentacyclic triterpene mono and diesters of Calendula officinalis flowers by non-aqueous C30 HPLC and hyphenation with APCI-QTOF-MS. J Pharm Biomed Anal. 2016; 118: 195-205. https://doi.org/10.1016/j.jpba.2015.10.025 CR - [12] Agatonovic-Kustrin S, Ramenskaya G, Kustrin E, Morton, DW. Characterisation of α-amylase inhibitors in marigold plants via bioassay-guided high-performance thin-layer chromatography and attenuated total reflectance-Fourier transform infrared spectroscopy. J Chromatog B. 2021; 1173: 122676. https://doi.org/10.1016/j.jchromb.2021.122676 CR - [13] Guidance for Industry, Bioanalytical method validation, US Department of Health and Human Services, Food and Drug Administration. CDER, Rockville MD, 2001. https://doi.org/10.1016/j.ica.2020.119681 CR - [14] Text on Validation of Analytical Procedures Q2A, International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use, London, 1994. CR - [15] Serim E, Ceylan B, Tekkeli-Kepekci SE. Determination of apigenin in cosmetics containing chamomile by high-performance liquid chromatography with ultraviolet detection (HPLC-UV). Anal Lett. 2023; 56(13): 2113-2122. http://dx.doi.org/10.1080/00032719.2022.2155180 UR - https://doi.org/10.12991/jrespharm.1734461 L1 - https://dergipark.org.tr/en/download/article-file/5021463 ER -