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1.
淫羊藿炮制前后UPLC-PDA-MS的指纹图谱研究 总被引:2,自引:0,他引:2
建立了朝鲜淫羊藿和柔毛淫羊藿药材的超高效液相色谱(UPLC)指纹图谱分析方法,实验结果表明,两个品种的指纹图谱差别较大,朝鲜淫羊藿标出35个共有峰,质谱鉴定了26个峰,柔毛淫羊藿标出13个共有峰,质谱鉴定了9个峰;研究了朝鲜淫羊藿和柔毛淫羊藿炮制前后UPLC指纹图谱的变化规律,指纹图谱发生了五处变化.该法快速、简便,重现性好,从整体上显示淫羊藿药材和炮制品的特征,为淫羊藿的生品和炮制品的质量控制提供了有效手段. 相似文献
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淫羊藿属药材反相高效液相色谱指纹图谱及质量评估研究 总被引:6,自引:0,他引:6
用一种新的多台阶梯度洗脱的反相高效液相色谱(RPLC)法, 首次建立了秦岭山区产4种产地及亚属均不相同的淫羊藿属药材的由9种成分组成的色谱指纹图谱. 并以淫羊藿甙为内标作为相对标准, 对其质量进行了评估. 然而, 因其产地和亚属的不同, 指纹图谱又各有特征, 发现产地不同的两种淫羊藿亚属, 箭叶淫羊藿的RPLC指纹图谱由12个色谱峰组成. 还提出用相对含量比较法对各种类淫羊藿中9种成分的含量进行了质量评价. 本工作所建立的淫羊藿属药材的RPLC指纹图谱法从试样提取的精密度、稳定性、图谱重复性等方面均符合《中药注射剂指纹图谱研究的技术要求(暂行)》中的有关规定. 该方法具有重现性好, 特征性强, 方法简便、快速等特点, 有可能成为淫羊藿药材种属判断、质量评估的标准, 也会对未来开发淫羊藿中其他有效成分提供科学的依据. 相似文献
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朝鲜淫羊藿中一种黄酮醇甙的化学结构 总被引:2,自引:0,他引:2
朝鲜淫羊藿中一种黄酮醇甙的化学结构李文魁,肖培根,廖矛川,张如意(中国协和医科大学药用植物研究所,北京,100094)(北京医科大学药学院)关键词朝鲜淫羊藿,黄酮醇甙,结构分析前文[1]中我们报道了从朝鲜淫羊藿(EpimediumkoreanumNa... 相似文献
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毛细管电泳法测定淫羊藿甙的pK_a值及其在中药淫羊藿中的含量 总被引:12,自引:2,他引:10
利用毛细管电泳中不同 pH条件下有效淌度 (μeff)与缓冲溶液中氢离子的浓度 ([H+])的非线性关系以及1/ μeff与缓冲溶液中 [H+]的线性关系 ,测定了淫羊藿甙的离子淌度 (μA- )和pKa 值 ;考察了在有机改性剂存在的情况下 ,随缓冲溶液中有机改性剂浓度的增加 ,淫羊藿甙的 pKa 值的变化情况。在缓冲溶液为V(2 4mmol/L磷酸盐 )∶V(乙醇 ) =70∶30时 ,对中药淫羊藿中淫羊藿甙的含量进行了定量测定 ,结果发现校正峰面积 (Y)与淫羊藿甙的质量浓度 (X ,g/L)的线性相关方程为Y =6 96× 10 -3 + 17 0X ,线性范围为 0 0 32g/L~ 0 35 4g/L。 相似文献
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离子液体提取分离鹿藿中异黄酮化合物 总被引:6,自引:1,他引:5
以1-丁基-3-甲基咪唑四氟硼酸盐([Bmim]BF4)离子液体取代天然产物研究中的溶剂,对具有抗雄性生育活性和抑菌作用的鹿藿根中的异黄酮成分进行提取和分离。 从鹿藿根的70%乙醇粗提物中,成功分离纯化得到3种异黄酮类化合物,它们均是首次从植物鹿藿中分离得到。 经过波谱分析鉴定,3种化合物的结构被确定为木豆酮(Cajanone)、鸡豆黄素A(Biochanin A)和1种新的异黄酮类化合物,被命名为3-[4′-(1″-甲氧基)-丙基氧代]-苯基-5,7-二羟基异黄酮(3-[4′-(1″-methoxy)propoxy]-phenyl-5,7-dihydroxy-isoflavone)。 建立了植物鹿藿中异黄酮含量的测定方法:以木豆酮化合物为标准品,在其紫外最大吸收峰270 nm处,测得生药中总异黄酮的含量为0.73%;测得平均加样回收率99.94%,相对标准偏差3.66%,离子液体回收率76.7%。 相似文献
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朝鲜淫羊藿的色谱指纹图谱及液相色谱/电喷雾串联质谱分析 总被引:1,自引:0,他引:1
建立了长白山区朝鲜淫羊藿药材的高效液相色谱指纹图谱的分析方法. 确定了18批朝鲜淫羊藿药材的13个共有峰, 该指纹图谱的精密度、稳定性和重现性的相对标准偏差均低于3.0%. 结合液相色谱/电喷雾串联质谱对特征峰进行了结构确认, 并根据电喷雾串联质谱数据推测了13个特征化合物的结构. 结果表明采用高效液相色谱与质谱联用技术对朝鲜淫羊藿色谱指纹图谱中的特征峰进行结构确认, 使其色谱指纹图谱的特征性更强, 更适合于药材质量的鉴别与评价. 相似文献
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HPLC法同时测定淫羊藿中朝藿定A、B、C与淫羊藿苷的含量 总被引:8,自引:0,他引:8
建立了同时测定淫羊藿中朝藿定A、B、C与淫羊藿苷含量的高效液相色谱方法。淫羊藿样品经超声波提取,以50%(φ)乙醇溶液为溶剂,在温度50℃、料液比1∶60条件下超声波提取30 m in,共提取2次。色谱条件:ZORBAX SB-C8色谱柱(5μm,4.6×250 mm);流动相A为乙腈,B为1%乙酸溶液;梯度洗脱;紫外检测波长为270 nm。上述4种类黄酮的标准曲线在6.6~33.0 mg/L(朝藿定A、淫羊藿苷)或6.6~55.0mg/L(朝藿定B、C)范围内呈良好的线性关系(r>0.99);加标回收率在97%~102%之间;相对标准偏差小于2%(n=5)。测得不同产地心叶淫羊藿叶片中4种类黄酮的质量分数差异较大;朝藿定A广泛分布于淫羊藿属中。本方法在淫羊藿药材质量控制中具有一定的参考价值。 相似文献
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ZHANG Gai LIANG Yong-Qing ZHANG Rong-Lan ZHANG Wei-Hai ZHAO Jian-She GUO Zhi-An 《结构化学》2005,24(7):783-789
A new quinazolinone compound 2,3-dihydro-2-(2-hydroxyphenyl)-3-phenylquinazolin-4(IH)-one 3 ([C2oH16O2N2]-C2H5OH, Mr = 362.42) and compound 2-(2-hydroxybenzylidene-amino)-N-phenyl-benzamide 2 (C2oH16O2N2, Mr = 316.34) were prepared from a precursor of 2-amino-N-phenyl-benzamide 1 (C13H12ON2, Mr = 212.25). Compound 3 was characterized by single-crystal X-ray diffraction analysis. The crystal belongs to orthorhombic,space group Pbca with a = 1.2889(11), b = 1.6170(14), c = 1.7729(15) nm, V= 3.695(6) nm^3, Z= 8, F(000) = 1536, Mr = 362.42, Dc = 1.303 g/cm^3, μ(MoKa) = 0.087 mm^-1, R = 0.0447 and wR= 0.0879. The crystal structure analysis indicates that the title compound has a two-dimensional network structure formed by hydrogen bonds and electrostatic interactions. 相似文献
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配合物形成的三维超分子体系—[Ni(C_6H_4O_2N)_2(H_2O)_4]的水热法合成、晶体结构及热分析 总被引:7,自引:0,他引:7
采用水热法用Ni(NO3)26H2O和异烟酸制备出了一种新的由配合物形成的三维超分子体系—[Ni(C6H4O2N)2(H2O)4],并通过X射线衍射对其晶体结构进行了测定。 该晶体属三斜晶系,空间群为Pī, 所得晶胞参数为: a = 6.9228(4), b = 9.6664(19),c = 6.322(1) , a = 96.86(3), b = 113.33(3), g = 110.35(3)°, V = 347.6(1) 3, Z = 1, Mr = 374.98, Dc = 1.791 g/cm3, F(000) = 194, m = 1.443 mm-1。用1362个可观察的 (I > 2s(I))衍射点,修正123个结构参数, 最终偏离因子R = 0.0444,wR = 0.1271。在组成该化合物的基本结构单元[Ni(C6H4O2N)2(H2O)4]中,Ni处于1个稍微拉长的八面体的中心; 各个结构单元之间通过氢键OH…O相互连接,形成了无限伸展的具有层状结构的三维超分子体系。 另外,从差热及热重曲线可以看出,该化合物加热到154 ℃时开始分解, 首先失去4个H2O,再失去2个异烟酸根,最后残余物为NiO。 相似文献
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Philip J. Cox James L. Wardell 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(8):o515-o517
The molecular structure of the title compound, C20H24B2N2O2S, is characterized by a twofold rotation axis passing through the S atom and the midpoint of the C—C single bond in the thiophene ring. A coordinative NB bond is present in the boroxazolidine ring and a single N—H?O hydrogen bond [H?O 1.93 (3) Å, N?O 2.829 (3) Å and N—H?O 172 (2)°] links the molecules into a molecular ladder. 相似文献
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新颖的咪唑官能化夹心型钨铋酸盐超分子化合物的合成与晶体结构 总被引:2,自引:2,他引:0
在常规条件下合成了一个新颖的超分子化合物Na8H[{Na(H2O)}3{Mn(C3H4N2)}3(BiW9O33)2]·32H2O, 通过X射线单晶结构分析、红外光谱及元素分析对该化合物进行了表征. 结果表明, 该化合物属六方晶系, P6(3)/m空间群. 晶胞参数a=1.394 8(4) nm, b=1.394 8(4) nm, c=3.348 6(19) nm, γ=120°, V = 5.641(4) nm3, Z=12. 该化合物是以α-B-BiW9钨铋酸盐为基本构筑单元的夹心结构化合物. 夹层中心3个Mn2+分别与3个咪唑分子配位形成无机-有机杂化材料. 3个[{Na(H2O)}3{Mn(C3H4N2)}3(BiW9O33)2]9-多阴离子结构基元利用氢键(非典型氢键)沿ab面构筑成具有三角形空穴的二维层状骨架结构. 这种二维层状结构利用氢键作用沿c轴方向交错排列, 形成了含有一维六边形孔道的三维超分子结构. 相似文献
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以5-氯吡嗪-2-羧酸甲酯和水合肼为原料,经亲核取代和脱水缩合反应合成了3种新型吡嗪类碳酰肼化合物C13H14N6O(a)、C13H14N6O2(b)和C12H12N6O2(c)。采用元素分析与核磁共振氢谱对化合物a~c进行了表征,结果表明合成的产物即为目标化合物。通过溶剂挥发法培养得到了化合物a的单晶并利用X-射线单晶衍射测定化合物a的晶体结构为单斜晶系。根据紫外-可见光谱可知,化合物a~c均以插入模式与CT-DNA作用。利用微量热实验测定了化合物a~c与CT-DNA的相互作用,发现反应过程放热,热效应ΔH依次为-5.77×103、 -5.50×103和-5.96×103 kJ·moL-1,反应时间均小于40 min。通过分子对接模拟计算明确了化合物a和b与DNA的具体结合位点包括A链DC4和DG5以及B链DC4、 DG5和DA6,化合物c与DNA的具体结合位点包括A链DC4和DG5以及B链DC4和DG5。采用牛津杯法测定了化合物a~c对枯草芽孢杆菌、金黄色葡萄球菌、铜绿假单胞菌以及大肠杆菌四种细菌的抑菌活性,结果表明化合物a~c均对铜绿假单胞菌表现出优于阳性对照组四环素的抑菌活性。 相似文献
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1-Allyl- (2) and 7-allyl-6-amino-3-methyl-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H)-one (3) were obtained via the 18-crown-6-ether catalyzed room temperature reaction of 6-amino-3-methyl-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H)-one (1) with potassium carbonate and allyl bromide in dry acetone. The structures of these two derivatives were verified by 2D-NMR measurements, including gHSQC and gHMBC measurements. The minor compound 2 may possess aromatic character. A single crystal X-ray diffraction experiment indicated that the major compound 3 crystallizes from dimethyl sulfoxide in the monoclinic space group P2(1)/n and its molecular structure includes an attached dimethylsulfoxide molecule, resulting in the molecular formula C(10)H(16)N(6)O(2)S. Molecular structures of 3 are linked by extensive intermolecular N-H...N hydrogen bonding [graph set C(1)(1)(7)]. 1 Each molecule is attached to the dimethyl sulfoxide oxygen via N-H...O intermolecular hydrogen bonding. The structure is further stabilized by pi-pi stacking interactions. 相似文献
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《结构化学》1989,(3)
<正> The preparation and molecular structure of the novel five-coordinate zinc compound CZn(C4H13N3) (C2H3O2)]ClO4(Mr= 327. 04) are described. The crystal belongs to orthorhombic space group Pn21a with a=8. 352(2) ,6=8. 642(2) ,c=17. 758 (4)A,V=1282A3,Z=4,0c=1.69gcm-3,Dm=1.70gcm-3,F(000) = 672,u(MoKa)= 22.01cm-1.The complex cation has a distorted trigonal bipyramidal geometry wifr each acetat anion C2H3O2- bridging two zinc atoms so that a chain structure along a axis is formed by the complex cations [Zn(C4H13N3)(C2H3O2)]+. 相似文献
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Benzotriazole,N,N’-dimethylpiperazine and N-methylpiperazine were applied to crystallize with 5-sulfosalicylic acid(5-H2SSA),affording three new binary molecular cocrystals [(C6H6N3+).(C7H5O6S-)].H2O(1),[(C6H16N22+)1/2.(C7H5O6S-)].H2O(2) and [(C5H14N22+).(C7H5O6S-)2].3H2O(3) under general conditions.Proton-transferring occurs from acid to nitrogen of N-donor compounds in all compounds 1,2 and 3.Analysis of the hydrogen-bonding synthons and their effects on crystal packing were also presented in the context of crystal engineering and host-guest chemistry.In compound 1,1-D infinite chains are extended to a 2-D layered architecture via strong O-H...O hydrogen bonds and then to a 3-D network by N-H...O interactions.Compound 2 and 3 both have the 1-D chain which is formed by O-H...O bonds and weak C-H...O hydrogen bonds.A common intramolecular S(6) [synthon I] ring is formed by the hydroxyl with the carboxyl group in all three compounds. 相似文献
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Miras HN Raptis RG Lalioti N Sigalas MP Baran P Kabanos TA 《Chemistry (Weinheim an der Bergstrasse, Germany)》2005,11(8):2295-2306
Reaction of NH4VO3 with sulfur dioxide affords the hexanuclear cluster (NH4)2(Et4N)[(V(IV)O)6(mu4-O)2(mu3-OH)2(mu3-SO3)4(H2O)2]Cl x H2O (1), and the decapentanuclear host-guest compound (Et4N)5{Cl subset [(VO)15(mu3-O)18(mu-O)3]} x 3 H2O (2). Sequential addition of magnesium oxide to an acidic aqueous solution of NH4VO3 (pH approximately 0) followed by (NH4)2SO3 resulted in the formation of either the non-oxo polymeric vanadium(IV) compound trans-(NH4)2[V(IV)(OH)2(mu-SO3)2] (3) or the polymeric oxovanadium(IV) sulfite (NH4)[V(IV)O(SO3)1.5(H2O)] x 2.5 H2O (4) at pH values of 6 and 4, respectively. The decameric vanadium(V) compound {Na4(mu-H2O)8(H2O)6}[Mg(H2O)6][V(V)10(O)8(mu6-O)2(mu3-O)14] x 3 H2O (5) was synthesised by treating an acidic aqueous solution of NH4VO3 with MgO and addition of NaOH to pH approximately 6. All the compounds were characterised by single-crystal X-ray structure analysis. The crystal structure of compound 1 revealed an unprecedented structural motif of a cubane unit [M4(mu4-O)2(mu3-OH)2] connected to two other metal atoms. Compound 3 comprises a rare example of a non-oxo vanadium(IV) species isolated from aqueous solution and in the presence of the reducing agent SO3(2-), while compound 4 represents a rare example of an open-framework species isolated at room temperature (20 degrees C). In addition to the synthesis and crystallographic studies, we report the IR and magnetic properties (for 1, 2 and 3) of these vanadium clusters as well as theoretical studies on compound 3. 相似文献
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合成了[CH3(C6H4)N2O(C6H4)COO(C6H4)OCH2Si(CH3)2]2O,经IR,1^HNMR和元素分析表征,并测定其单晶结构。结果表明,晶体属单斜晶系,空间群为P21/c,晶胞参数a=1.7557(1),b=1.0938(9),c=2.3300(1)nm,β=105.6(6)°,V=4.3116nm^3,Mr=855.07,Z=4,Dc=1.317g/cm^3,μ(CuKα)=6.335cm^-1,F(000)=900,最终的偏离因子R=0.0837,Rw=0.0913。该分子中,柔性的四甲基二硅氧烷嵌段与氧化偶介晶基团形成ABA结构齐聚物。两条刚性的介晶基链节的轴向几乎平行向上伸出。径长比(L/D)为4.23.该液晶化合物的要变温度K174.4N226.8Ⅰ.通过结构分析,讨论了该类化合物的结构对液晶相变行为的影响。 相似文献