高效液相色谱法测定痹祺胶囊中马钱子碱、士的宁和丹酚酸B

建立了同时测定痹祺胶囊中马钱子碱、士的宁和丹酚酸B含量的方法.采用反相高效液相色谱法,色谱柱:Inertsil ODS-3(250 mm×4.6 mm,5 μm);流动相:V(乙腈): V(10 mmol/L己烷磺酸钠的磷酸盐缓冲液,pH 2.86)=22: 78;流速: 1.0 mL/min;检测波长: 254 nm;柱温:25 ℃.马钱子碱、士的宁和丹酚酸B的线性范围分别为2.7～32 mg/L(r=0.9998)、2.6～31 mg/L(r=0.9999)和12.7～151 mg/L(r=0 9991);平均加样回收率(n=6)分别为99.3%、95.6%和98.9%;RSD分别为2.30%、3.68%和1.82%.本方法简便快捷,结果准确,可用于痹祺胶囊的质量控制.     

高效液相色谱法同时测定参茸补酒中芍药苷、阿魏酸的含量

建立一种高效液相色谱双波长法同时测定参茸补酒中芍药苷、阿魏酸的含量。该方法采用Symmetry C18色谱柱(150×3.9mm,5μm),流动相为乙腈 水 冰乙酸(12∶88∶1,V/V),检测波长分别为323nm(通道1)、230nm(通道2)。结果显示:芍药苷、阿魏酸分别在21.4～214.0和1.65～16.50μg·mL-1范围内本法有良好的线性关系;平均回收率分别为98.1%(RSD=1.28%)和97.5%(RSD=1.73%)。本法操作简便,快速,重现性好,结果准确,可作为参茸补酒的质量控制方法。     

高效液相色谱法测定贯叶连翘中的4种成分

本文利用高效液相色谱法同时测定中药贯叶连翘中绿原酸、芦丁、金丝桃苷和槲皮素四种成分的含量。采用Tiahhe Kromasil C18 100 A(5μm,250mm×4.6 mm)反相色谱柱;流动相为V(乙腈)∶V(水)=20∶80(含0.02%三氟乙酸);紫外检测波长270nm;流速1.0 ml/min;柱温40℃。绿原酸、芦丁、金丝桃苷和槲皮素线性范围分别为3.4~34μg.mL-1(r=0.9993),1.8~18μg.mL-1(r=0.9998),2.3~23μg.mL-1(r=0.9999),3.5~35μg.mL-1(r=0.9991),平均回收率(n=5)分别为98.4%(RSD=1.48%),101.8%(RSD=0.74%),103.7%(RSD=0.77%),103.5%(RSD=1.28%)。方法线性范围宽、相对标准偏差低、精密度高、重现性好,应用于贯叶连翘及制剂样品的测定,结果令人满意。     

RP-HPLC法测定复方丹参片中的隐丹参酮、丹参酮Ⅰ和丹参酮ⅡA

建立了反相高效液相色谱法测定复方丹参片(丹参、三七、冰片)中的隐丹参酮、丹参酮Ⅰ和丹参酮ⅡA。采用DiamonsilTMC18(250×4.6 mm,5μm)色谱柱,以V(甲醇)∶V(水)=75∶25为流动相,流速为0.8 mL/min,检测波长270nm。隐丹参酮、丹参酮Ⅰ和丹参酮ⅡA分别在1.456~10.19μg/mL、2.160~15.12μg/mL和3.152~22.06μg/mL的范围内呈良好线性关系,平均回收率分别为99.21%(RSD=0.63%)、100.3%(RSD=1.0%)、99.87%(RSD=0.63%)。可用于复方丹参片的质量控制。     

高效液相色谱法测定富含油脂辣椒制品中的辣椒素类物质

建立了高效液相色谱法测定高油脂辣椒制品中3种主要辣味成分的方法.样品以70%乙醇提取,采用反相高效液相色谱分离,紫外检测器;根据色谱峰的保留时间定性,以外标峰面积法定量辣椒素(C)、二氢辣椒素(DC)、去甲二氢辣椒素(NDC),结果以斯氏指数(SHU)计.NDC的色谱行为与C极其类似,NDC可采用C的标准曲线定量.采用色谱柱,ZORBAX SB-C18;流动相,V(甲醇)∶V(水)=70∶30;UV检测波长,230 nm;辣椒素和二氢辣椒素RSD分别为1%,1.5%(n=5);回收率分别为97.5%、94.5%.辣椒素和二氢辣椒素在0.001～0.1 mg/mL范围内线性良好;LOD 0.1 mg/L,LOQ 0.5 mg/L.供试品溶液稳定,12 h内测定RSD为1%.方法满足辣味水平评价要求.     

HPLC测定云雾龙胆花中獐牙菜苷和异荭草苷的含量

建立云雾龙胆花中獐牙菜苷和异荭草苷含量测定的HPLC方法。采用微波辅助动态回流法进行提取,色谱条件:Fusion-RP 80 A C18柱(150×4.6 mm,5μm);流动相:甲醇-0.2%磷酸溶液梯度洗脱(0~20 min∶18∶82~30∶70;20~30min∶30∶70~40∶60;30~35min∶40∶60~50∶50);流速:1 mL/min;柱温:30℃;检测波长254 nm。云雾龙胆花中獐牙菜苷和异荭草苷的色谱峰与共存组分完全达到基线分离,线性范围分别为0.25~1.25μg(r=0.9998),0.432~2.160μg(r=0.9999),平均加样回收率分别为97.7%(RSD=0.84%),99.2%(RSD=0.76%)。     

塞曼火焰原子吸收法测定黄河水体的总硬度

采用原子吸收分光光度法测定黄河水体的总硬度,钙的浓度在0.100～5.00 mg/L、镁的浓度在0.0500～2.00 mg/L范围内分别与吸光度呈线性关系,线性方程分别为A=0.045 5c+8.354×10~(-5)、A=0.514c+8.354×10~(-5),相关系数均为0.9999。黄河水样6次测定结果的相对标准偏差为1.2％,t检验结果表明,该法与EDTA络合滴定法测定结果无显著性差异。     

高压液相色谱法测定马铃薯叶提取物中茄尼醇的含量

首次采用高压液相色谱法测定马铃薯叶提取物中茄尼醇的含量。条件为:Hypersil C18色谱柱,流动相为V(甲醇)∶V(乙醇)=80∶20,流速为1.0mL/min,紫外检测波长为215 nm,柱温30℃。实验结果表明,该方法在茄尼醇进样量1.3~4.6μg时具有良好的线性关系(Y=1685.1X 10.358,R=0.9996);加样回收实验(n=5)的平均回收率为98.2%,RSD为1.32%。     

高效液相色谱法测定杜仲叶中的绿原酸

 采用高效液相色谱法测定杜仲叶中绿原酸的含量。所用色谱柱为Shim-packCLC-ODS柱,以巯嘌呤为内标,以甲醇-0.01mol/L磷酸二氢钾缓冲液(体积比为25∶75;pH3.9)为流动相,UV检测波长为328nm。在上述色谱条件下,当绿原酸质量浓度为25～300mg/L时,以绿原酸对照品溶液与内标液的峰面积比为纵坐标(Y),绿原酸的质量浓度为横坐标(X),二者呈良好的线性关系,线性方程为Y=8.0368X+1.275×10-3,r=0.9999;平均回收率为99.89%,RSD=1.45%(n=6)。     

高效液相色谱-荧光检测法测定环境水中的苯胺和苯酚

建立了用高效液相色谱荧光检测法同时测定环境水中苯胺和苯酚的分析方法。色谱柱为EclipseXDB C8(4.6mmi.d.×150mm,5μm),流动相为甲醇 磷酸盐缓冲液(0.1mol/L磷酸二氢钾 0 1mol/L磷酸氢二钠,pH6.87)V(甲醇)∶V(磷酸盐缓冲液)=50∶50,流速1 0mL/min,柱温25℃,检测波长0minλex/λem=230/340nm(测定苯胺),3.5minλex/λem=215/300nm(测定苯酚)。测定苯胺的线性范围0.2～120ng,r=0.9999,检出限0.01ng;测定苯酚的线性范围0.4～500ng,r=0.9998,检出限0.02ng,回收率98.1%～101.2%。该方法已用于对环境水中苯胺和苯酚的测定。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.