Name 2,3,5,4\'-tetrahydroxystibene-2-o-β-d-glucoside
Appearance Brown yellow
CAS No. 82373-94-2
Formulae
Molecular Weight 406.38
Natural Resources
Synonyms
Bioactivities
Identification
1HNMR
13CNMR
Analytical Method
INSTRUMENT Silica Gel G plate
MOBILE PHASE Benzene: ethyl acetate: Formic acid = 5: 5: 2
DETECTION UV λ365 nm
INSTRUMENT SHIMADAZU LC-10A HPLC
COLUMN Spherigel C18 column, 5Lm, 4.6 x 150 mm, 30°C
MOBILE PHASE Acetonitrile: water = 17: 83, 1.0 mL/min
DETECTION UV λ320 nm
INSTRUMENT Shimadzu LC-2010C HT system and Shimadzu HPLC workstation (Shimadzu, Japan)
COLUMN Shimadzu VP-ODS column (150 mm × 4.6 mm I.D., 5 μm) at room temperature
MOBILE PHASE A: methanol, B: water, 0-60 min 5-100% A
DETECTION UV λ254 nm
INSTRUMENT Waters Acquity™ Ultra Performance LC system (Waters, USA)
COLUMN ACQUITY UPLC BEH C18 column (2.1 × 100 mm, 1.7 µm, UK), 40°C
MOBILE PHASE A: 0.1% v/v formic acid in water, B: acetonitrile, 0-0.5 min 1% B, 0.5-10 min 1-20% B 10-12 min, 20-90% B 12-15 min 90-1% B, and 15-16 min 1% B, 0.5 mL/min
DETECTION Waters Xevo™ QTof MS (Waters), a quadrupole and orthogonal acceleration TOF-MS (Waters), which was equipped with a LockSpray™ interface and an ESI source. Nebulizer and auxiliary gas: nitrogen, collision gas: argon, negative ion mode, ESI capillary voltage: 2.5 kV, source and desolvation: 120 and 450°C, desolvation and cone gas: 700 and 30 L/h.The sample cone: 40 V, extraction cone: 4.0 V, lockspray capillary: 2.0 kV. The collision energy: 30-45 eV.
Sample Preparation
METHOD 1
Sample extracted with 5 L 95% ethanol to form syrup, and was dissolved in 300 ml of water by sonication and partitioned with ether and n-butanol of equal volume three times. n-butanol was loaded on D-101 macroporous resin column (35 cm × 3.4 cm, the volume of the column was 170 ml) and eluted with 1700 ml of distilled water and 3400 ml of 30% ethanol. The ethanol part is prepared for separation.
TBE-300 high-speed counter-current chromatography (Tauto Biotechnique, Shanghai, China) with three multilayer coil separation column connected in series (I.D. of the tubing = 1.5 mm, total volume = 300 ml) and a 20 ml sample loop and a S-1007 constant flow pump (Shenyitong Tech & Exploitation, Beijing, China), a Model 8823B-UV monitor (Bingdayingchuang Sci & Tech, Beijing, China). The data were collected with model N2000 chromatography workstation (Zhejiang University, Hangzhou, China)
Ethyl acetate: methanol: water = 50: 1: 50, v/v/v, mobile phase: lower phase
2.0 mL/min, 800 rpm
Shimadzu LC-2010C HT system and Shimadzu HPLC workstation (Shimadzu, Japan) with Shimadzu VP-ODS column (150 mm × 4.6 mm I.D., 5 μm) at room temperature, A: methanol, B: water, 0-60 min 5-100% A, UV λ254 nm
Reference
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