求翻译!!
(Figure1(b)).Amongthem,theABTSassay(Figure1(c))showedthatFr.9hasbyfarthestrongestacti...
(Figure 1(b)). Among them, the ABTS assay
(Figure 1(c)) showed that Fr.9 has by far the
strongest activity. Fr.9 was further purified to yield
compound 1.
ThepositiveAPCI-ITMSspectrumofCompound1
showed a protonated molecular ion peak at m/z 127
t
[M t H] .Soitsmolecularweightwasdeterminedto
1
be 126. The H-NMR spectrum (Table I) of 1
(500MHz, methanol-d4) showed two cis-olefinic
proton signals at dH 7.94 (1H, d, J 1/4 5.5Hz) and
6.39(1H,d,J 1/4 5.5Hz).Inaddition,thesignalofone
methylgroupdirectlyattachedtoanolefiniccarbonat
13
dH 2.35 (3H, s) was observed. The C-NMR
spectrum(TableI)showedonecarbonylcarbonsignal
atdC175.3,andfourolefiniccarbonsignalsatdc156.3,
152.2, 144.6 and 114.4, indicating the presence of a
pyranone ring. The signal at dc 14.2 corresponded to
thecarbonofthemethylgroup.Compound1wasalso
analyzed by HPLC-DAD. Its retention time and UV
spectra(absorptionmaximaat210and275nm)agreed
verycloselywiththoseobtainedfromauthenticmaltol.
So the MS spectrum, NMR data, the retention time
andUVspectrumsupporttheidentityofcompound1
as 3-hydroxy-2-methyl-4H-pyran-4-one (maltol)
(Figure 2).
Fractions 1–8 and 10 were also analyzed by APCI-
ITMS, suggesting these fractions contain molecules
with molecular weight ranging from 124 to 214 (data
not shown).
Content of maltol and its contribution to the TAA of dark
soy sauce
A considerable part of the TAA of the DSS was
contained in MeOH-R and EtOAc-R fractions and in
fractions 1–8 and 10 (Figure 1). Although maltol was
identified as the active fraction of Fr. 9, we needed to
determine its overall contribution to TAA. Thus an
HPLC method was developed for determination of
maltol in DSS.
Maltol standard was dissolved in methanol-0.1%
formic acid (10:90, v/v) yielding concentrations of
0.25, 0.5, 1.0, 1.5, 2.0mM. Three different sets of
standard solutions were prepared and analyzed each
day and in three continuous days. Calibration curves
for the quantification of maltol were obtained by
plotting concentration (mM) against peak area. 展开
(Figure 1(c)) showed that Fr.9 has by far the
strongest activity. Fr.9 was further purified to yield
compound 1.
ThepositiveAPCI-ITMSspectrumofCompound1
showed a protonated molecular ion peak at m/z 127
t
[M t H] .Soitsmolecularweightwasdeterminedto
1
be 126. The H-NMR spectrum (Table I) of 1
(500MHz, methanol-d4) showed two cis-olefinic
proton signals at dH 7.94 (1H, d, J 1/4 5.5Hz) and
6.39(1H,d,J 1/4 5.5Hz).Inaddition,thesignalofone
methylgroupdirectlyattachedtoanolefiniccarbonat
13
dH 2.35 (3H, s) was observed. The C-NMR
spectrum(TableI)showedonecarbonylcarbonsignal
atdC175.3,andfourolefiniccarbonsignalsatdc156.3,
152.2, 144.6 and 114.4, indicating the presence of a
pyranone ring. The signal at dc 14.2 corresponded to
thecarbonofthemethylgroup.Compound1wasalso
analyzed by HPLC-DAD. Its retention time and UV
spectra(absorptionmaximaat210and275nm)agreed
verycloselywiththoseobtainedfromauthenticmaltol.
So the MS spectrum, NMR data, the retention time
andUVspectrumsupporttheidentityofcompound1
as 3-hydroxy-2-methyl-4H-pyran-4-one (maltol)
(Figure 2).
Fractions 1–8 and 10 were also analyzed by APCI-
ITMS, suggesting these fractions contain molecules
with molecular weight ranging from 124 to 214 (data
not shown).
Content of maltol and its contribution to the TAA of dark
soy sauce
A considerable part of the TAA of the DSS was
contained in MeOH-R and EtOAc-R fractions and in
fractions 1–8 and 10 (Figure 1). Although maltol was
identified as the active fraction of Fr. 9, we needed to
determine its overall contribution to TAA. Thus an
HPLC method was developed for determination of
maltol in DSS.
Maltol standard was dissolved in methanol-0.1%
formic acid (10:90, v/v) yielding concentrations of
0.25, 0.5, 1.0, 1.5, 2.0mM. Three different sets of
standard solutions were prepared and analyzed each
day and in three continuous days. Calibration curves
for the quantification of maltol were obtained by
plotting concentration (mM) against peak area. 展开
1个回答
展开全部
图1(b))。其中,ABTS测试(图1(c))表明,Fr.9迄今为止最强的。 Fr.9产量进一步纯化化合物1。 ThepositiveAPCI - ITMSspectrumofCompound1显示,在m / z127吨[米T H]条。Soitsmolecularweightwasdeterminedto 1质子化分子离子峰是126。在H - NMR谱(见表一)1(500MHz的,甲醇4点)展示了两个顺式烯质子信号,在卫生署7.94(1小时,D,J升1 / 4 5.5Hz)和6.39(1小时,D,J升1 / 4 5.5Hz)。Inaddition,thesignalofone methylgroupdirectlyattachedtoanolefiniccarbonat卫生署13 2.35(3小时,S)的观察。这架C - NMR谱(TableI)showedonecarbonylcarbonsignal atdC175.3,andfourolefiniccarbonsignalsatdc156.3,152.2,144.6和114.4,表明一个吡喃环存在。在直流信号相当于14.2 thecarbonofthemethylgroup.Compound1wasalso的HPLC - DAD的分析。其保留时间和紫外光谱(absorptionmaximaat210and275nm)同意verycloselywiththoseobtainedfromauthenticmaltol。因此,在MS谱,核磁共振数据,保存时间andUVspectrumsupporttheidentityofcompound1为3 -羟基- 2 -甲基- 4小时-吡喃4一(麦芽酚)(图2)。馏分1-8和10人还分析了大气压化学电离ITMS,表明这些馏分分子含有124至214不等的重量(未显示)分子。麦芽醇及其贡献,黑酱油的TAA一对直资塔阿相当部分的内容载于甲醇- R和乙酸乙酯- R的组分及组分1-8和10(图1)。尽管麦芽酚被确定为神父的活性部位。 9,我们需要确定其整体贡献塔阿。因此,一个开发了高效液相色谱法测定麦芽酚在决策支持系统。麦芽酚标准溶解于甲醇-0.1%甲酸(10:90,v / V选择)0.25,0.5,1.0,1.5,2.0毫米高产浓度。三组不同的标准解决方案的编制和分析每一天,在连续三次天。通过绘制校准曲线,对峰浓度(毫米)面积得到了量化的麦芽酚
已赞过
已踩过<
评论
收起
你对这个回答的评价是?
推荐律师服务:
若未解决您的问题,请您详细描述您的问题,通过百度律临进行免费专业咨询