Jieyun Huang

Volatile components of Rhizoma Alpiniae Officinarum using three different extraction methods combined with gas chromatography–mass spectrometry

Volatile components from Rhizoma Alpiniae Officinarum were respectively extracted by three methods including hydrodistillation, headspace solid-phase microextraction (HS-SPME) and diethyl ether extraction. A total of 40 (hydrodistillation), 32 (HS-SPME) and 37 (diethyl ether extraction) compounds were respectively identified by gas chromatography–mass spectrometry (GC/MS) and 22 compounds were overlapped, including α-farnesene, γ-muurolene, 2,6-dimethyl-6-(4-methyl-3-pentenyl)bicyclo[3.1.1]hept-2-ene, eucalyptol and cadina-1(10), 4-diene and so forth, varying in relative contents. HS-SPME is fast, sample saving and solvent-free and it also can achieve similar profiles as those from hydrodistillation and solvent extraction. Therefore, it can be the priority for extracting volatile components from medicinal plants.

ISOLATION AND PURIFICATION OF PAEONIFLORIN AND ALBIFLORIN FROM RADIX PAEONIAE RUBRA BY HIGH-SPEED COUNTER-CURRENT CHROMATOGRAPHY

Paeoniflorin and albiflorin were isolated and purified from Radix Paeoniae Rubra by high-speed counter-current chromatography with a solvent system of ethyl acetate-n-butanol-water (3:2.5:5, v/v/v) in one step. From 100 mg of the n-butanol extract of Radix Paeoniae Rubra, 10 mg of paeoniflorin and 4.3 mg of albiflorin were obtained with purity of 98.75% and 95.03%, as determined by HPLC. Their structures were identified by MS, UV, and NMR analysis. In this study, a rapid method for isolation and purification of the two major compounds from Radix Paeoniae Rubra crude extract was established.

Isolation and Purification of Geniposide, Crocin-1, and Geniposidic Acid from the Fruit of Gardenia jasminoides Ellis by High-Speed Counter-Current Chromatography

Geniposide, crocin-1, and geniposidic acid were simultaneously separated from the fruit of Gardenia jasminoides Ellis by one step of high-speed counter-current chromatography with the solvent system composed of ethyl acetate-n-butanol-water(1:4:5, v/v/v) within 130 min. The purities of the three compounds were 98.7%, 97.1%, and 90.4%, respectively, as determined by HPLC. Their structures were confirmed by MS, UV, 1H NMR, and13C NMR analysis.

ISOLATION AND PURIFICATION OF 20-HYDROXYECDYSONE FROM RADIX SERRATULAE CHINENSIS BY HIGH-SPEED COUNTER-CURRENT CHROMATOGRAPHY

□ The bioactive compound 20-Hydroxyecdysone was successfully isolated and purified from Radix Serratulae Chinensis by high-speed counter-current chromatography with a solvent system of ethyl acetate–n-butanol–water (4:1:5, v/v/v) in one step. From 230mg of the n-butanol extract of Radix Serratulae Chinensis, 16.7mg of 20-Hydroxyecdysone was obtained with purity of 99.3%, as determined by high performance liquid Chromatography (HPLC). The structure was identified by mass spectrophotometry (MS), ultraviolet spectrophotometry (UV), and nuclear magnetic resonance spectrophotometry (NMR) analysis. In this study, a rapid method for isolation and purification of the major compound from Radix Serratulae Chinensis extract was established.

Separation and Purification of Arctiin, Arctigenin, Matairesinol, and Lappaol F from Fructus Arctii by High-Speed Counter-Current Chromatography

Arctiin (I), arctigenin (II), matairesinol (III), and lappaol F (IV) were isolated and purified from the traditional Chinese medicine Fructus Arctii by high-speed counter-current chromatography (HSCCC). The crude extracts from Fructus Arctii were treated with D101 macroporous resin first and divided into two parts: fraction 1 and fraction 2. Fraction 1 was separated by ethyl acetate-n-butanol-water (4:0.5:5, v/v/v) and yielded 164 mg of I from 250 mg of fraction 1. Fraction 2 was separated by n-hexane-ethyl acetate-methanol-water (2:3:2:3, v/v/v/v) and yielded 27 mg of II, 5 mg of III, and 3 mg of IV from 150 mg of fraction 2. The purities of the four compounds were 99.64%, 98.48%, 96.16%, and 91.41%, respectively, as determined by HPLC-DAD. The chemical structures of the isolated compounds were identified by MS, UV, 1H NMR, and 13C NMR analysis.

ISOLATION AND PURIFICATION OF FORSYTHOSIDE A AND SUSPENSASIDE A FROM FORSYTHIA SUSPENSA BY HIGH-SPEED COUNTER-CURRENT CHROMATOGRAPHY

Forsythoside A and suspensaside A were isolated and purified from Forsythia suspensa by one step of high-speed counter-current chromatography for the first time using a solvent system of ethyl acetate-n-butanol-methanol-water (4:0.5:0.5:5, v/v). The purities of the two compounds were 98.19% and 98.05%, respectively, as determined by HPLC. Their structures were identified by MS, UV, and NMR analysis. Such a simple and effective method was fairly useful to prepare pure compounds as reference substances for related study on Forsythia suspensa.

Preparative isolation and purification of 12,13-dihydroxyeuparin from Radix Eupatorii Chinensis by high-speed counter-current chromatography

An efficient method for the isolation and purification of 12,13-dihydroxyeuparin from Radix Eupatorii Chinensis by high speed counter-current chromatography (HSCCC) was established in this paper. The ether extracts of Radix Eupatorii Chinensis were purified by HSCCC with a solvent system of hexyl hydride–ethyl acetate–methanol–water (1:2:1:2, v/v/v/v). The upper phase was used as the stationary phase and the lower phase as the mobile phase. About 8.4 mg of 12,13-dihydroxyeuparin was obtained from 200 mg of ether extracts from Radix Eupatorii Chinensis in one-step HSCCC separation, with the purity of 96.71%, as determined by HPLC. After methanol–water recrystallization, the purity of 12,13-dihydroxyeuparin reached 99.83%. Such a simple and effective method was fairly useful to prepare pure compound as reference substances for related study on Radix Eupatorii Chinensis.

Isolation and Purification of Isoquercitrin and Quercitrin from sf Hypericum Japonicum Thunb.ex Murray by Counter-Current Chromatography

Isoquercitrin and quercitrin were successfully isolated and purified from Hypericum japonicum Thunb.ex Murray by counter-current chromatography with a solvent system of n-hexane-ethyl acetate-methanol-water (1:7:1:7, v/v/v/v) in one step. From 100 mg of the extract of Hypericum japonicum Thunb.ex Murray, 9.8 mg of isoquercitrin and 12 mg of quercitrin were obtained with the purities of 95.9% and 99.1%, respectively, as determined by HPLC. Their structures were identified by UV, MS, and NMR analysis. In this study, a rapid method for isolation and purification of the two major compounds from Hypericum japonicum Thunb.ex Murray crude extract was established.

PREPARATIVE ISOLATION OF TETRANDRINE AND FANGCHINOLINE FROM RADIX STEPHANIA TETRANDRA USING REVERSED-PHASE FLASH CHROMATOGRAPHY

Tetrandrine and fangchinoline were successfully separated by reversed-phase flash chromatography on a manually-packed C18 column from Radix Stephania tetrandra. After recrystallization by acetone, 13 mg of fangchinoline and 21 mg of tetrandrine were obtained from 100 mg Stephania tetrandra extract, with their relative content 98.78% and 98.19%, respectively. Their structures were characterized by UV, IR, MS, and NMR. The established method was simple, fast, and reproducible, which can be applied to the preparation of reference substances of tetrandrine and fangchinoline.

ISOLATION AND PURIFICATION OF ECHINACOSIDE AND ACTEOSIDE FROM CISTANCHE TUBULOSA (SCHRENK) WIGHT BY HIGH-SPEED COUNTER-CURRENT CHROMATOGRAPHY

Echinacoside and acteoside were isolated and purified from Cistanche tubulosa (Schrenk) Wight by one step of high-speed counter-current chromatography for the first time using a solvent system of ethyl acetate-n-butanol-glacial acetic acid-water (1:1.2:0.2:2, v/v/v/v). The experiment yielded 16.9 mg of echinacoside and 5.1 mg of acteoside from 220 mg of Cistanche tubulosa (Schrenk) Wight extract. The purity of the two compounds was 99.14% and 95.04%, respectively, as determined by HPLC. Their structures were identified by MS, UV, IR, and NMR analysis. Such a simple and effective method was fairly useful to prepare pure compounds as reference substances for related study on Cistanche tubulosa (Schrenk) Wight.