| Abstract [eng] |
Research aim – to analyze and compare the peculiarities of the composition of silimarin in a range of commercial preparation with a variety of milk thistle preparations. Research goals: 1. to determine and compare the quantitative composition of silymarin commercial phytopreparations by high performance liquid chromatographic analysis; 2. to analyze and compare the composition of phenolic compounds of silymarin preparations by ultra highperfomance liquid chromatography – tandem mass spectrometry. Research objective. 10 herbal products containing silymarin were investigated. The study was performed by analyzing the composition of herbal food supplements and medicinal preparations in the assortiment of the Lithuanian pharmacies supply. Selected preparations contain extracts of Silybum Marianum L. 5 – one component preparations were selected for the study, and 5 multicomponent preparations. Of these, 5 over-the-counter medications and 5 dietary supplements were selected. Research method. Ultra high performance liquid chromatography selected for the quantification of flavonolignans. The distribution of tests samples and monitoring of deviations in the concentration of silymarin components were performed by the ultra high performance liquid chromatography method. The mobile phase gradient was used for the separation of analytes. Mobile phase A eluent was: deionized water. Another mobile phase B eluent was the mixture of: phosporic acid R, methanol R, and water R (0.5:35:65 V/V/V). The area of the analytical peaks was used for quantitative processing. Repeatibility of the test for eah solution was 3 times. Qualitative testing of phytopreparations by ultra-eficient liquid chromatogaphy-tandem mass spectrometry also was performed. The chromatographic peaks of the flavonoids obtained during the study were identified by the retention time (Rt) of the analyte and the reference compound and the mass spectra of analytes obtained with a mass spectrometric detector. Chromatographic peaks were identified using multiple reaction monitoring (MRM) and scanning modes. Research results and conclusion. After examination of the constituents of the herbal preparations, the test solutions, in particular the efficient tandem mass spectrometric methods for liquid chromatography, relating to all the most appropiate methods. The following compounds were also identified: over-the-counter drug (1) – quinic acid, 3,4-dihydroxibenzoic acid, ferulic acid, dicapheoylquinic acid, kemferol-3-O-glucoside, apigenin-7-glucoside, eriodicitol, quercetin derivatives, kemferol, pinocembrin, chrysine, over-the-counter drug (2) – quinic acid, dicapheoylquinic acid, quercetin-7-glucoside, taxifoline, apigenin-7-glucoside, eriodicitol, quercetin derivatives, chemferol, pinocembrin, chrysine, dietary supplements (3) – quinic acid derivatives, sinapic acid, taxifoline, apigenin-7-glucoside, eriodictiol, quercetin, pinocembrin, chrysine, dietary supplements (5) – quinic acid derivatives, 3,4-dihydroxybenzoic acid, chlorogenic acid, coffee acid derivatives, kemferol-3-O-glucuronide, taxifoline, kemferol-3-O-glucoside, florizine, eriodicitol, myricetin, quercetin, isoramnetin, pinocembrin. The ultra high performace liquid chromatography method was applied for 10 commercial herbal products containing silymarin. Comparison of the quantitative parameters of silymarin revealed that the lignanoflavone profile varied. The sum of silibinin A and B was found to range from 54,69 proc. to 67,06 proc. of total amount of all flavonolignans. The highest percentage of the sum of silibinin A and silibinin B was found in the test sample (3) of the over-the-counter herbal medicine. Based on the amount of silymarin per dosage unit specified by the phytopreparator manufacturer, the compliance of the obtained quantitative indicators with the labeling was assessed and it was found that the variation in phytochemical composition is characteristic of silymarin products. |
