Agilent 1200, 测定糖类用什么柱子

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Mass spectrometry
An Agilent XCT Plus ion trap mass spectrometer
(ITMS)(AgilentTechnology,US)wasusedtoanalyze
the fractions, Fr. 1–10, obtained from ethyl acetate
extracts. Atmospheric pressure chemical ionization
(APCI) MS was performed in the positive mode. The
dry gas and vaporiser temperatures were 350 and
4008C, respectively.
For the analysis of CP1, Electrospray-Ionization
Mass Spectrometry (ESI-MS) was performed using a
Waters Micromass Q-Tof micro mass spectrometer
(Waters,USA).Samplewasdirectlyinfusedataspeed
of 10ml/min for acquiring mass spectra. The capillary
and sample cone voltages were maintained at 3.0kV
and 50V, respectively. The source and desolvation
temperatures were 80 and 2508C, respectively. The
mass spectra were acquired from m/z 100 to 5000 in
the positive ion mode.
Nuclear magnetic resonance spectrometry (NMR)
The NMR spectra of compound 1, CP1 and CP2
were recorded on a Bruker Advance AMX500 NMR
spectrometer(Rheinstetten, Germany) at500.13MHz
1 13
( H)and125.75MHz( C),respectively.Tetramethyl-
silane (TMS) was used as an internal standard.
Compound 1 was dissolved in methanol-d4; CP1 and
CP2weredissolvedinD2O.
Statistical analysis
The mean values were calculated from data taken
from at least three separate experiments. Where
significance testing was performed, a Student’s t-test
was used; P-values of ,0.05 were considered to be
statistically significant.
Results
No significant differences in TEAC value or HPLC
profile were detected between different bottles of the
same commercial batch. The antioxidant components
in DSS were found to be stable during 1–2 months
storage, based on the TEAC value and their HPLC
profile.
Separation and characterization of low molecular mass
components
DSS was extracted with methanol, and the methanol
extract was further partitioned with ethyl acetate as
described in Material and Methods. The three
fractions of DSS, MeOH-R, EtOAc-extract and
EtOAc-R were subjected to the ABTS assay. The
MeOH-Rfraction contributed about 60%of the TAA
of DSS. However, the EtOAc-extract showed the