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The possibilities in the identification and quantitation of the constituents of Rubia tinctorum L.'s root, called also madder root, was described and compared by gas chromatography (GC)-MS, high-performance liquid chromatography (HPLC)-UV/photodiode array detection (DAD) and HPLC-MS: chromatographic analyses were carried out in parallel, from the same samples/extracts/hydrolyzates. Anthraquinone glycosides, anthraquinones, carboxylic acids and sugars were determined directly in the presence of the matrix and in its extracts without and subsequently to hydrolyses. Hydrolyses were performed as a function of time, with hydrochloric and trifluoroacetic acids, as well as enzymatically. Data revealed that as hydrolyzing agent trifluoroacetic acid is to be preferred. Madder root's anthraquinones (pseudopurpurin/purpurin, alizarin, lucidin, munjistin, nordamnacanthal) were identified on the basis of their absorption spectra (HPLC-DAD) and fragmentation patterns by GC-MS and HPLC-MS, equally. Reproducibility of anthraquinone's quantitation, by HPLC-DAD and GC-MS, in the concentration ranges of 4 x 10(-5) to 3 x 10(-2)g/g dried sample, provided an average reproducibility of 4.2% (varying between 0.9 and 9.4% relative standard deviation (RSD percentages)). Carboxylic acids (malic, citric, quinic, rosmarinic acids) and saccharides (xylose, ribose, fructose, glucose, sucrose, primverose) were quantified as their trimethylsilyl (oxime) ether/ester derivatives by GC-MS, in the concentration ranges of 10(-5)g to 10(-2)g/g dried sample, with an average reproducibility of 4.7% RSD.

In this paper we identify/determine the composition of the extracts of Dracocephalum moldavica L. and D. ruyschiana L. with special emphasis on their flavonoids, aliphatic, aromatic carboxylic acids and sugars. The plant materials were extracted using methanol-acetone 1:1 (v/v) acidified with HCl (0.05%). Composition of extract's most red fractions was identified by HPLC, while the constituents of the entire extract were identified and quantified as their trimethylsilyl-(oxime) ether/ester derivatives by GC-MS. On the basis of HPLC analyses - (performed on Phenomenex Luna 5 µm C18 column, 250× 4.6 mm I.D.; eluent: acetonitrile - trifluoroacetic acid (0.1 %); isocratic/gradient conditions) - delphinidin, cyanidin and pelargonidin (in traces) were identified by spectral analysis and on the basis of authentic standard's addition. GC-MS analyses were carried out immediately with extracts, as well as subsequently to extract's hydrolysis (trifluoroacetic acid: 2M, 2h, 4h). Constituents were identified and quantified as their trimethylsilyl-(oxime) ether/ester derivatives, from a single run, on the basis of their total (TIC) and selective fragment ion (SIM) responses. Calculations were related to the dry matter content of extracts. As main constituents monosaccharides, sugar alcohols di- and trisaccharides, aliphatic (phosphoric, succinic, levulinic, malic, tartaric, fatty acids) and aromatic (quinic, chlorogenic, caffeic, ferulic, 3,4-dihydroxyphenyllactic, rosmarinic) carboxylic acids and their corresponding esters; apigenin, luteolin flavon aglycons and tocopherol, in total 33 constituents were quantitated partly by their TIC, partly by their SIM responses. Identification/quantification proved to be in total of 35–69% (expressed in the dry matter content of extracts).