| Summary: | Three phenylethanoid glycosides, echinacoside (<b>1</b>), salidroside (<b>3</b>), and acteoside (<b>6</b>), and three secoiridoid glycosides, isonuezhenide (<b>2</b>), nuezhenoside G13 (<b>4</b>), and specnuezhenide (<b>5</b>), have been extracted and separated by a combined method of ultrahigh pressure extraction (UPE) and high-speed counter-current chromatography (HSCCC) from Ligustri Lucidi Fructus. For the UPE, the optimal extraction was developed with conditions including solvent of 90% ethanol, sample to solvent ratio of 1:20 g/mL, pressure of 200 MPa, and time of 2 min, which rendered the yields of compounds <b>4</b> and <b>5</b> were 15.0 and 78.0 mg/g, respectively. For the HSCCC separation, the strategy of changing flow rates between 1.0 and 2.0 mL/min allowed the acquisition for 2.7 mg of compound <b>1</b>, 4.5 mg of compound <b>2</b>, 6.8 mg of compound <b>3</b>, 5.9 mg of compound <b>4</b>, 11.2 mg of compound <b>5</b>, and 2.2 mg of compound <b>6</b> in one separation run under the solvent system of ethyl acetate:<i>n</i>-butanol:water (2:1:3, <i>v</i>/<i>v</i>) from 200 mg of the UPE extract. The structures of these phenylethanoid and secoiridoid glycosides were elucidated by extensive spectroscopic methods.
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