ABSTRACT
A validated analytical method is reported for the analysis of paeoniflorin and albiflorin in Bai Shao (Paeonia lactiflora) as a dried raw herb and commercially prepared dried aqueous extract. The samples were extracted by sonication in methanol and the extract analyzed by LC-photodiode array with identity confirmation by electrospray ionization-tandem MS. A C18 column was used with an acetonitrile-water gradient mobile phase. Paeoniflorin and albiflorin were quantified at 230 nm. Ions with m/z 121 and 327 were produced with the MS detector, using the paeoniflorin precursor ion with m/z 479. For albiflorin, the precursor ion with m/z 479 produced the m/z 121 and 77 ions. The amounts of paeoniflorin and albiflorin found in the raw herb were 33.2 and 1.8 mg/g, respectively; and in the dried aqueous extract, the amounts were 34.8 and 15.7 mg/g, respectively. The LODs for paeoniflorin and albiflorin were 0.37 and 1.39 mg/g, respectively, for the raw herb and 0.25 and 0.06 mg/g, respectively, for the dried aqueous extract.
Subject(s)
Benzoates/analysis , Bridged-Ring Compounds/analysis , Glucosides/analysis , Paeonia/chemistry , Chromatography, Liquid , Chromatography, Thin Layer , Indicators and Reagents , Medicine, Chinese Traditional , Monoterpenes , Plant Extracts/analysis , Plant Preparations/analysis , Reference Standards , Solvents , Spectrometry, Mass, Electrospray Ionization , Spectrophotometry, UltravioletABSTRACT
Vaccinium myrtillus or bilberry fruit is a commonly used herbal product. The usual method of determining the anthocyanin content is a single-wavelength spectrophotometric assay. Using this method, anthocyanin levels of two extracts were found to be 25% as claimed by the manufacturers. When high-performance liquid chromatography (HPLC) was used, however, one extract was found to contain 9% anthocyanins probably not derived from V. myrtillus but from an adulterant. This adulterant was subsequently identified, using HPLC, mass spectroscopy, and nuclear magnetic resonance, as amaranth, that is, 3-hydroxy-4-[(4-sulfo-1-naphthalenyl)azo]-2,7-naphthalenedisulfonic acid trisodium salt-a synthetic dark red sulfonic acid based naphthylazo dye. As described in this study, if deliberate adulteration occurs in an extract, a single-wavelength spectrophotometric assay is inadequate to accurately determine the levels of compounds such as anthocyanins. Detection of deliberate adulteration in commercial samples thus requires the use of alternative, more sophisticated, methods of analysis such as HPLC with photodiode array detection as a minimum.
Subject(s)
Amaranth Dye/analysis , Food Contamination/analysis , Fruit/chemistry , Vaccinium myrtillus/chemistry , Anthocyanins/analysis , Chromatography, High Pressure Liquid , Hydrogen-Ion Concentration , Magnetic Resonance Spectroscopy , Mass SpectrometryABSTRACT
The aerial parts of Zanthoxylum ovalifolium (Rutaceae) have yielded the two novel benzo[c]phenanthridine alkaloids terihanine (8-demethylnitidine) and isoterihanine (9-demethylnitidine) together with nitidine, the unusual furoquinoline 5-methoxydictamnine, canthin-6-one and several common furocoumarins. The finding of benzo[c]phenanthridine and furoquinoline alkaloids in Australian material of this species confirms its chemical homogeneity throughout its range from India to Australia.