2
018
H. Zhu et al. / Carbohydrate Research 346 (2011) 2016–2018
Table 3
GC–MS was performed using an Agilent 7890A gas chromato-
graph with a 5975C mass spectrometry detector. The temperature
m) was main-
tained at 50 °C for 3 min and then raised to 300 °C with a ramp rate
of 15 °C/min for 5 min. The flow rate of Helium was 1 mL/min with
the split ratio of 20:1.
a
Conversion of fructose in methanol–organic solvent system
b
b
Conversionb
(%)
Entry
V
Methanol/V(organic
Y
(%)
HMF
Y
(%)
MMF
Y
(%)
(HMF+MMF)
of the column (DB-5 ms, 50 m  250
l
m  0.25
l
solvent)
1
2
3
3/7
5/5
5/5
18.0
12.4
17.0
35.8
34.4
37.5
53.8
46.8
54.5
95.1
95.0
96.1
a
Acknowledgements
Reaction conditions: fructose 2 g; Amberlyst-15 0.30 g; 120 °C; 180 min reac-
tion time;
Vmethanol + V(organic solvent) = 10 mL. 1: acetone; 2: ethyl acetate; 3:
chloroform.
This workis supportedby theNationalHigh TechnologyResearch
and Development Program of China (No. 2009AA05Z410), the Natu-
ral Science Foundation of China (No. 20803038, 21003146), the Key
Science and Technology Program of Shandong Province (No.
2008GG20002038), and the Natural Science Foundation of Shan-
dong Province (No. ZR2010BQ014).
b
The HMF yield and fructose conversion were determined by HPLC.
1
1
. Experimental
.1. Materials and experimental procedures
Fructose (P99%) purchased from Solarbio Science & Technology
Supplementary data
Co., Ltd was used as a standard. 5-Hydroxymethylfurfural (P99%)
and 5-methoxymethylfurfural (P98%) obtained from WuJiang
YingChuang Chemical Reagent Co., Ltd were used as standards.
Anhydrous MeOH (P99.5%), acetone (P99.5%) and chloroform
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Ethyl acetate (P99.5%) and anhydrous diethyl ether were supplied
by Guangdong Guanghua Chemical Factory Co., Ltd. Amberlyst-15
was purchased from Sigma–Aldrich.
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