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HPLC测定长形肉豆蔻中赤式-6-澳白木脂素的含量 被引量:3
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作者 张萌萌 许枬 《中国药师》 CAS 2010年第11期1628-1630,共3页
目的:建立长形肉豆蔻中赤式-6-澳白木脂素含量的测定方法。方法:采用HPLC法,色谱柱为Kromasil C_(18)(250 mm×4.6 mm,5μm)。流动相为乙腈-水(65∶35);流速为1.0 ml·min^(-1);检测波长为228nm。柱温:25℃。结果:赤式-6-澳白... 目的:建立长形肉豆蔻中赤式-6-澳白木脂素含量的测定方法。方法:采用HPLC法,色谱柱为Kromasil C_(18)(250 mm×4.6 mm,5μm)。流动相为乙腈-水(65∶35);流速为1.0 ml·min^(-1);检测波长为228nm。柱温:25℃。结果:赤式-6-澳白木脂素在0.22~2.24 mg·ml^(-1)范围内线性关系良好,r=0.999 9。平均加样回收率为100.7%,RSD为2.71%(n=9)。结论:所建立的方法简单、准确、重复性好,可用于测定长形肉豆蔻中的赤式-6-澳白木脂素含量。 展开更多
关键词 长形肉豆蔻 赤式-6-澳白木脂素 高效液相 含量测定
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赤式-2-氨基-1-苯基-1-丙醇合成工艺改进 被引量:1
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作者 蔡小华 胡薇 姚祖凤 《中国药物化学杂志》 CAS CSCD 2002年第2期110-111,共2页
以苯丙酮为起始原料 ,经过羟亚氨基苯丙酮中间体和用Pt Pd/C作催化剂加氢反应合成赤式 2 氨基 1 苯基 丙酮 ,并对其工艺进行了改进 ,降低了成本 ,简化了工艺 ,提高了收率 ,总收率5 5 5 %。
关键词 苯丙酮 羟亚氨基苯丙酮 赤式-2-氨基-1-苯基-1-丙酮 合成
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赤式-2-(2,4-二氟苯基)-3-甲基-2-[(1H-1,2,4-三唑-1-基)甲基]环氧乙烷的合成 被引量:2
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作者 黄汉忠 李树军 《精细化工中间体》 CAS 2006年第3期14-15,18,共3页
以间二氟苯为原料,经傅克酰化、水解、环合等反应制得三唑丁醇类抗真菌药物的重要中间体赤式-2-(2,4-二氟苯基)-3-甲基-2-[(1H-1,2,4-三唑-1-基)甲基]环氧乙烷,总收率44.6%,纯度98%以上(HPLC),工艺稳定,利于工业生产。
关键词 赤式-2-(2 4-二氟苯基)-3-甲基-2-[(1H-1 2 4-三唑-1-基)甲基]环氧乙烷 化学合成 工艺研究 抗真菌药
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活性铋粉促进下3—溴环己烯和醛的高选择性赤式加成
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作者 任平达 邵东 《合成化学》 CAS CSCD 1997年第A10期600-600,共1页
关键词 铋粉 溴环己烯 高选择性 赤式加成
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构型转换法制备赤式紫胶桐酸及反应机理分析 被引量:2
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作者 石小娟 唐保山 +3 位作者 张雯雯 李坤 涂行浩 张弘 《精细化工》 EI CAS CSCD 北大核心 2021年第4期815-822,共8页
以苏式紫胶桐酸为原料,通过构型转换法制备赤式紫胶桐酸。采用FTIR、质谱、核磁(1HNMR/13CNMR)、TG、DSC、XRD、手性拆分、比旋光度等表征手段对所得产物进行了分析确证。对紫胶桐酸苏式到赤式构型的转换机理进行了初步探究。结果表明:F... 以苏式紫胶桐酸为原料,通过构型转换法制备赤式紫胶桐酸。采用FTIR、质谱、核磁(1HNMR/13CNMR)、TG、DSC、XRD、手性拆分、比旋光度等表征手段对所得产物进行了分析确证。对紫胶桐酸苏式到赤式构型的转换机理进行了初步探究。结果表明:FTIR、质谱、核磁显示,产物与苏式紫胶桐酸结构一致;XRD、DSC、TG结果表明,苏式紫胶桐酸与产物具有相同晶型,但产物熔点更高,晶胞尺寸更小;手性拆分结果显示,产物为紫胶桐酸的光学异构体,从而确定产物为赤式紫胶桐酸。对中间产物的结构表征表明,苏式紫胶桐酸到赤式紫胶桐酸构型转换的机理为卤素和羟基之间双分子亲核取代(SN2)和双分子消除反应(E2)同时发生的反应,羟基和卤素间的两次SN2反应是发生构型转换反应(Walden转换)的关键;羟基/卤素间的E2反应是苏式紫胶桐酸能够彻底转化为赤式紫胶桐酸的原因。 展开更多
关键词 紫胶桐酸 苏式 赤式 构型转换 机理 医药原料
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赤式2-氨基-1苯基-1-丙醇合成工艺改进
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作者 胡薇 蔡小华 《沈阳化工学院学报》 2001年第4期256-258,共3页
以苯甲醛和硝基乙烷为起始原料 ,经缩合 ,氧及催化加氢反应合成赤式 2 氨基 1 苯基 1 丙醇 ,并作出了工艺上的改进 .在缩合反应中 ,加入DMF作溶剂 ,产率提高 1 0 % ,反应时间缩短5 0h ,在催化加氢反应中 ,产率提高 5 % ,并讨论了... 以苯甲醛和硝基乙烷为起始原料 ,经缩合 ,氧及催化加氢反应合成赤式 2 氨基 1 苯基 1 丙醇 ,并作出了工艺上的改进 .在缩合反应中 ,加入DMF作溶剂 ,产率提高 1 0 % ,反应时间缩短5 0h ,在催化加氢反应中 ,产率提高 5 % ,并讨论了反应条件 ,本工艺的总收率 5 8% . 展开更多
关键词 2-硝基-1-苯基-1-丙醇 2-硝基-1-苯基-1-丙酮 赤式-2-氨基-1-苯基-1-丙醇 合成 工艺 肾上腺受体兴奋药
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赤式盐酸甲氧明结构表征研究
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作者 陈海龙 柯海媚 +2 位作者 钟武坤 何兆昌 岳峰 《广东化工》 CAS 2020年第14期38-39,共2页
本文阐述了采用X-射线单晶衍射法对赤式盐酸甲氧明结构表征的研究。晶体结构表明,赤式盐酸甲氧明属于单斜晶系,P21/c空间群,属于中心对称空间群两种对映异构体以1:1的比例排列,晶胞参数为a=14.3041(3),b=9.5298(2),c=9.6595(2),α=90... 本文阐述了采用X-射线单晶衍射法对赤式盐酸甲氧明结构表征的研究。晶体结构表明,赤式盐酸甲氧明属于单斜晶系,P21/c空间群,属于中心对称空间群两种对映异构体以1:1的比例排列,晶胞参数为a=14.3041(3),b=9.5298(2),c=9.6595(2),α=90°,β=99.302°,γ=90°,V=1299.42(5),Z=4,F(000)=660,R1=0.0389,wR2=0.1094。 展开更多
关键词 赤式盐酸甲氧明 X-射线单晶衍射 核磁共振
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紫胶皂化废液中回收紫胶桐酸工艺研究
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作者 王世贤 唐保山 +3 位作者 张弘 马金菊 刘兰香 徐涓 《林产化学与工业》 CAS CSCD 北大核心 2023年第5期56-62,共7页
为提高紫胶桐酸得率,以工厂制备紫胶桐酸所残留的紫胶皂化废液为原料,通过构型转化法经盐析、酸析、脱色、重结晶等步骤回收紫胶桐酸,通过单因素试验优化紫胶桐酸构型转化工艺,采用核磁、质谱、红外、热重对制备的紫胶桐酸结构进行分析... 为提高紫胶桐酸得率,以工厂制备紫胶桐酸所残留的紫胶皂化废液为原料,通过构型转化法经盐析、酸析、脱色、重结晶等步骤回收紫胶桐酸,通过单因素试验优化紫胶桐酸构型转化工艺,采用核磁、质谱、红外、热重对制备的紫胶桐酸结构进行分析,采用差示扫描量热、高效液相色谱C18柱拆分法等表征方法对制备的紫胶桐酸进行构型分析。研究结果表明:通过构型转化法回收紫胶桐酸可提高紫胶桐酸得率,确定了最佳制备条件为原料和浓盐酸的料液比3∶5(g∶mL)、反应温度100℃、反应时间7 h,活性白土用量为紫胶桐酸粗品质量的10%,活性白土脱色及使用20%乙醇溶液重结晶各2次后,所制备的紫胶桐酸得率为3.78%±0.5%,纯度为80.65%±0.41%。产物结构及构型分析结果表明:所制备的产物为赤式紫胶桐酸。该方法制备的紫胶桐酸来自废弃物,且精制后杂质较少,从而可有效提高紫胶桐酸得率。 展开更多
关键词 紫胶桐酸 构型转化 苏式构型 赤式构型
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天然有机化合物的质谱研究(Ⅶ)——直链邻二醇类化合物构型的确定 被引量:1
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作者 华苏明 李宏 +3 位作者 陈耀祖 李海泉 翟建军 陈能煜 《高等学校化学学报》 SCIE EI CAS 1988年第11期1126-1130,共5页
用硼酸三甲酯作反应试剂,以反应质谱法研究某些直链邻二醇类化合物的构型。实验结果表明:凡苏式构型的样品与硼酸三甲酯反应产生的特征离子丰度比均大于赤式构型的样品与其反应所产生的特征离子丰度比。由此可方便地利用反应质谱法来鉴... 用硼酸三甲酯作反应试剂,以反应质谱法研究某些直链邻二醇类化合物的构型。实验结果表明:凡苏式构型的样品与硼酸三甲酯反应产生的特征离子丰度比均大于赤式构型的样品与其反应所产生的特征离子丰度比。由此可方便地利用反应质谱法来鉴别该类化合物的苏、赤式构型。 展开更多
关键词 反应质谱法 天然产物 苏式构型 赤式构型
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反式-5-(4-氯苯基)-4-甲基-2-氧代噻唑烷酮的合成 被引量:1
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作者 钱鹏程 陈均志 陈帆 《精细化工》 EI CAS CSCD 北大核心 2011年第3期300-302,共3页
报道了一种合成噻螨酮关键中间体——反式-5-(4-氯苯基)-4-甲基-2-氧代噻唑烷酮的方法。以赤式-1-对氯苯基-2-氨基丙醇盐酸盐和二硫化碳为原料,在130℃下直接环合得到反式5-(4-氯苯基)-4-甲基-2-氧代噻唑烷酮,收率82%,色谱纯度99%;再经... 报道了一种合成噻螨酮关键中间体——反式-5-(4-氯苯基)-4-甲基-2-氧代噻唑烷酮的方法。以赤式-1-对氯苯基-2-氨基丙醇盐酸盐和二硫化碳为原料,在130℃下直接环合得到反式5-(4-氯苯基)-4-甲基-2-氧代噻唑烷酮,收率82%,色谱纯度99%;再经双氧水氧化得到噻螨酮关键中间体,收率84%,色谱纯度95%。该工艺流程经两步合成得到目标产物,简化了操作步骤,缩短了反应时间,避免了酸性废水的排放,符合绿色化工的要求。 展开更多
关键词 赤式-1-对氯苯基-2-氨基丙醇盐酸盐 反式-5-(4-氯苯基)4-甲基-2-氧代噻唑烷酮 噻螨酮关键中间体
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Spring Cold Bias of SST and Minimal Wind Mixing in the Equatorial Pacific Cold Tongue 被引量:1
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作者 LIN Peng-Fei LIU Hai-Long LI Chao ZHANG Xue-Hong 《Atmospheric and Oceanic Science Letters》 2010年第6期342-346,共5页
The authors investigate the relationship between bias in simulated sea surface temperature (SST) in the equatorial eastern Pacific cold tongue during the boreal spring as simulated by an oceanic general circulation ... The authors investigate the relationship between bias in simulated sea surface temperature (SST) in the equatorial eastern Pacific cold tongue during the boreal spring as simulated by an oceanic general circulation model (OGCM) and minimal wind mixing (MWM) at the surface. The cold bias of simulated SST is the greatest during the boreal spring, at approximately 3℃. A sensi- tivity experiment reducing MWM by one order of magnitude greatly alleviates cold biases, especially in March-April. The decrease in bias is primarily due to weakened vertical mixing, which preserves heat in the uppermost layer and results in warmer simulated SST. The reduction in vertical mixing also leads to a weak westward current in the upper layer, which further contributes to SST warming. These findings imply that there are large uncertainties about simple model parameters such as MWM at the oceanic surface. 展开更多
关键词 cold biases the equatorial Pacific cold tongue the minimal wind mixing
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Removal of SO_2 from flue gas using Bayer red mud:Influence factors and mechanism 被引量:7
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作者 TAO Lei WU Heng +3 位作者 WANG Jie LI Bin WANG Xue-qian NING Ping 《Journal of Central South University》 SCIE EI CAS CSCD 2019年第2期467-478,共12页
The absorbent composing of Bayer red mud and water was prepared and applied to removing SO2 from flue gas.Effects of the ratio of liquid to solid(L/S),the absorption temperature,the inlet SO2 concentration,the O2 conc... The absorbent composing of Bayer red mud and water was prepared and applied to removing SO2 from flue gas.Effects of the ratio of liquid to solid(L/S),the absorption temperature,the inlet SO2 concentration,the O2 concentration,SO4^2-and other different components of Bayer red mud on desulfurization were conducted.The mechanism of flue gas desulfurization was also established.The results indicated that L/S was the prominent factor,followed by the inlet SO2 concentration and the temperature was the least among them.The optimum condition was as follows:L/S,the temperature and the SO2 concentration were 20:1,25℃and 1000 mg/m^3,respectively,under the gas flow of 1.5 L/min.The desulfurization efficiency was not significantly influenced when O2 concentration was above 7%.The accumulation of SO4^2-inhibited the desulfurization efficiency.The alkali absorption and metal ions liquid catalytic oxidation were involved in the process,which accounted for 98.61%. 展开更多
关键词 Bayer red mud flue gas desulfurization wet catalytic oxidation iron catalysis
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Evaluation of Baishao(Radix Paeoniae Alba)and Chishao(Radix Paeoniae Rubra)from different origins based on characteristic spectra of amino acids 被引量:1
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作者 LI Shasha ZHANG Yiping +4 位作者 DENG Yuanhui WANG Qian XIE Zhiru Ibarra-Estrada Emmanuel XIAO Xue 《Digital Chinese Medicine》 2021年第2期120-129,共10页
Objective To evaluate the difference between Baishao(Paeoniae Radix Alba,PRA)and Chishao(Paeoniae Radix Rubra,PRR)from different regions based on the characteristic spectra of amino acids(AAs).Methods Fingerprints of ... Objective To evaluate the difference between Baishao(Paeoniae Radix Alba,PRA)and Chishao(Paeoniae Radix Rubra,PRR)from different regions based on the characteristic spectra of amino acids(AAs).Methods Fingerprints of the 21 standard AAs were established using O-phthalaldehyde-9-fluorenylmethyl chloroformate(OPA-FMOC)pre-column derivation method.The AA components in PRA and PRR were characterized qualitatively and quantitatively,and different AAs were screened using pattern recognition technology.Results Twelve AAs were identified in both PRA and PRR.Meanwhile,aspartic acid,glutamic acid,arginine,alanine,and gamma-aminobutyric acid were screened as characteristic components,and their concentrations could effectively distinguish PRA from PRR.Conclusion The established characterization method,which is based on the characteristic spectra of AAs,is accurate,efficient,and sensitive and can effectively distinguish between PRA and PRR from different producing areas,thus providing a reference for the overall characterization and evaluation of Chinese medicinal materials. 展开更多
关键词 O-phthalaldehyde-9-fluorenylmethyl chloroformate(OPA-FMOC)pre-column derivatization method Amino acids characteristic spectra Baishao(Paeoniae Radix Alba PRA) Chishao(Paeoniae Radix Rubra PRR) Pattern recognition
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Mineralogy and textural impact on beneficiation of goethitic ore
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作者 Dey Shobhana Mohanta Manoj K. Singh Ratnakar 《International Journal of Mining Science and Technology》 SCIE EI CSCD 2017年第3期445-450,共6页
The effect of mineralogy and texture on the beneficiation of goethitic ores from two different origins is highlighted. Sample A having 54.47% Fe with 8.57% loss of ignition (LOl) indicates the presence of vitreous a... The effect of mineralogy and texture on the beneficiation of goethitic ores from two different origins is highlighted. Sample A having 54.47% Fe with 8.57% loss of ignition (LOl) indicates the presence of vitreous and ochreous goethite, martite and microplaty hematite as the major minerals. Sample B contains 56.90% Fe with 14.4% LOI. There is a pisolithic laterite containing vitreous and ochreous goethite, quartz, kaolinitic clay and there is no hematite mineral. The liberated minerals in -150 + 100 μm size class are 74% for Sample A and 37% only for Sample B which shows that the Sample A appears to be more amenable to beneficiate. A concentrate of 46.7% with 63.22% Fe could be recovered from Sample A while subjected to gravity separation followed by wet magnetic separation. The Sample B does not respond to gravity and magnetic separation due to its complex mineralogy. However, calcination of the Sample B followed by magnetic separation gives the encouraging results. Thus, anomalous behaviour of the goethite dominated ores in beneficiation is attributed to the different textural and liberation characteristic. 展开更多
关键词 Texture Pisolitic Ochreous goethite Vitreous goethite Calcination
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Metallothioneins Induced by Antimony Accumulation in Earthworm Eisenia foetida Using Filter Paper Contact Method
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作者 Mengjiao Geng Shuxuan Liang Wei Liu Kai Wang Hanwen Sun 《Journal of Environmental Science and Engineering(A)》 2013年第11期686-691,共6页
MTs (Eiseniafoetida metallothioneins) have been recently reported as biomarkers for environmental metal contamination, however no study regarding Sb (antimony) is available. This study aimed to explore possibility... MTs (Eiseniafoetida metallothioneins) have been recently reported as biomarkers for environmental metal contamination, however no study regarding Sb (antimony) is available. This study aimed to explore possibility of MTs as a biomarker of Sb pollution. A contact method of filter paper was used to investigate Sb inducing MTs in Eiseniafoetida. Spectrophotometrical and SDS-PAGE (sodium dodecyl sulphate-polyacrylamide gel electropheresis) analyses were used to determine the nature of the induced MTs samples. Rabbit liver metallothioneins was used as a standard. The results showed that the molecular weight of induced protein was approximately 6-7 kDa. A characteristic absorption peak at 268 nm was observed, which was consistent with the standard. The amounts of Sb-MTs quantified by cadmium hemoglobin saturation method showed a significant positive relationship with increasing Sb exposure.The experiments prove that Sb can induce Sb-MTs in Eiseniafoetida as a biomarker of antimony pollution. 展开更多
关键词 METALLOTHIONEINS Sb(III) Eiseniafoetida.
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ANTI-SADDLES OF A POLYNOMIAL SYSTEM
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作者 YE YANQIAN (Departmellt of Mathematics, Naming University, Naming 210008, China.) 《Chinese Annals of Mathematics,Series B》 SCIE CSCD 1995年第4期453-458,共6页
By using the generalized PoincarE index theorem it is proved that if the n2 critical points of an n-polynomial system form a configuration of type (2n -1) - (2n - 3) +(2n- 5) -…+ (- 1 )n- 1, and the 2n -1 outmost ant... By using the generalized PoincarE index theorem it is proved that if the n2 critical points of an n-polynomial system form a configuration of type (2n -1) - (2n - 3) +(2n- 5) -…+ (- 1 )n- 1, and the 2n -1 outmost anti-saddles form the venices of a convex (2n -1)-polygon, then among these 2n-1 anti-saddles at least one must be a node. 展开更多
关键词 Polynomial system Anti-saddle Poincare index theorem Equator.
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