A fast solid phase extraction-high performance liquid chromatography-ion trap mass spectrometry (SPE-HPLC-MSn) method is presented for quantitative determination of 3-(3,4-dihydroxyphenyl)-2-hydroxylpropionic acid (Danshensu, DSS) from Compound Danshen Dripping Pills (CDDP) in rabbits' heart, liver, kidney, and lung and for qualitative analysis of the bioactive metabolites of Radix Salvia miltiorrhizae (DS) from CDDP in these tissues. The proposed method was validated with a detection limit of 0.06 ng/mL and a linear range of 5.0-200 ng/mL for DSS. The main metabolites of DS were pyrocatechol, vanillic acid, isopropyl 3-(3,4-dihydroxyphenyl)-2-hydroxypropanoate, and 2-hydroxyl-3-(3,4-dihydroxyphenyl)propinonic sulfuric anhydride. In vitro pharmacological experiments demonstrated that isopropyl 3-(3,4-dihydroxyphenyl)-2-hydroxypropanoate had a distinct vasodilatating action.

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SummaryRetention volumes (VN) of different kinds of test compound have been measured on silica gel as a function of column temperature (T) in the range 20 to 210 ~ n-Heptane and mixtures of n-heptane and polar modifiers were used as mobile phases. With nC7 and nC7-1,4-dioxane mixtures, there was a good linear relationship between In VN and lIT for column temperatures above 100 ~ When more polar modifiers such as butanol, ethanol and acetic acid were used, 'N'-shaped curves were obtained for the plots of in VN against 1/T. Possible explanations of this retention behavior have been proposed on the basis of related studies and common physical chemistry relationships. Column equilibration time after alteration of water content or column temperature is greatly reduced at elevated temperatures. This will benefit the application of LSC on silica gel.