A reliable LC-MS method has been applied for the separation and identification of major constituents of the rhizome of Smilacis glabrae. Identification of the constituents was carried out by interpretation of their retention time, and MS and MS/MS data, especially by comparing these with Sarcandra glabra under the same LC-MS conditions, as well as the data provided by the literature. Thirty-three compounds, including catechin derivatives, flavanonols, phenolic acid derivatives and phenylpropanoid glycosides were either identified or tentatively characterized. Among them, compound 12 was deduced to be a new phenylpropanoid-substituted catechin. Fragmentation behaviors of the three major categories of compounds were also investigated. This UPLC-PDA/ESI-MS n method was effective for the separation and identification of the constituents and could be the basis for the comprehensive quality control of Smilacis glabrae.
The Ga(III)-7-iodo-8-hydroxyquinoline-5-sulfonic acid complex in the presence of suitable micelles and with sodium sulfite as oxygen scavenger exhibited strong phosphorescence at room temperature in aqueous solutions. This micellar reaction provides the basis for a convenient phosphorimetric determination of traces of gallium. Different types of micelles showed their maximum enhancing effects at different pH ranges, affording greater convenience for various analytical purposes. A phosphorimetric procedure with surfactant cetyltrimethylammonium bromide as enhancing agent is proposed. The detection limit for gallium was 5 ng/ml and the calibration graph was rectilinear in the range of 5 to 600 ng/ml. The relative standard deviation was 4% at 50 ng/ml level. The applicability of this room-temperature phosphorimetric procedure to multi-component analyses for the group III elements, AI(III), Ga(III), and In(III), was demonstrated. Kalman filtering was used to deconvolute the phosphorescence spectra of mixtures of aluminium and gallium allowing the simultaneous determination of both metals with satisfactory results.
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