N—羟基琥珀酰亚胺—间于甲氨基苯甲酸酯柱前衍生HPLC分离荧光检测？…

用Ｎ－羟基琥珀酰亚胺－间二甲氨基苯甲酸酯为柱前衍生试剂,Ｃ１８柱,含ｐＨ为４．０为１０ｍｍｏｌ／Ｌ柠檬酸－磷本氢二钠缓冲溶液的４０％的甲醇－水（Ｖ／Ｖ）溶液为流动相,反相高效液相色谱（ＲＰ－ＨＰＬＣ）分离荧光检测了氨、甲胺和乙胺,检出限分别为５．０、０．５和１．０ｐｍｏｌ,方法简便、快速。     

3,4′-二甲氧基莰菲醇的合成

以间苯三醛和茄香醛为原料,经Ｈｏｅｓｃｈ－Ｈｏｕｂｅｎ反应,羟基保护、缩合、Ａｌｇａｒ－Ｆｌｙｎｎ－Ｏｙａｍａｄｅ反应、甲基化、等６步反应合成了３,４′－二甲氧基莰菲醇。     

毛细管电泳在拮抗药物对氨基苯甲酸，对羟基苯甲酸和磺胺分析测…

本报道了一种用毛细管区带电泳法分离与测定对氨基苯甲酸、对羟基苯甲酸及磺胺类药物的新方法。电泳条件为：用２０ｍｍｏｌ／Ｌ硼砂－２０ｍｍｏｌ／ＬＨ３ＰＯ４－２０ｍｍｏｌ／Ｌβ－环糊精－４％乙醇作电泳液，Ｌ－抗坏血酸为内标，２８０ｎｍ为检测波长，样品由电进样方式１０ｋＶ／１０ｓ）引入毛细管（５１．２ｃｍ×５０μｍｉ．ｄ．，有效分离长度为３８．５ｃｍ）．在２４．５℃下，６ｍｉｎ内三可达基线分离（电泳电     

用气相色谱-原子发射光谱法检测VX、Bz及其降解产物

应用气相色谱－原子发射光谱（ＧＣ－ＡＥＤ）同时检测Ｓ－（２－二异丙基氨乙基）甲基硫直膦酸乙酯（ＶＸ）、二苯羟乙酸－３－喹咛环酯（ＢＺ）战剂及其降解产物等５种化合物,得取了Ｃ、Ｈ、Ｓ、Ｎ、Ｏ、Ｐ６种元素色谱图,通过选择合适的检测元素,其检出限ＶＸ为１５．６ｍｇ／Ｌ,Ｂｚ为１６．７９ｍｇ／Ｌ,二异基氨基乙太醇为３．０２ｍｇ／Ｌ,３－羟基喹咛为２８．４０ｍｇ／Ｌ,二苯羟乙酸甲酯为３１．７８ｍｇ／Ｌ,定量     

反相高效液相色谱法快速测定大麦籽粒中13种酚酸类化合物

建立了快速测定大麦籽粒中13种酚酸类化合物(没食子酸、原儿茶酸、绿原酸、对羟基苯甲酸、咖啡酸、香草酸、丁香酸、间羟基苯甲酸、对香豆酸、阿魏酸、藜芦酸、邻香豆酸和水杨酸)的反相高效液相色谱方法.采用SUPELCOAscentis(@) C18色谱柱(150 mm×4.6 mm,5μm)分离,流动相为甲醇-0.1％甲酸水溶...     

柱前衍生反相高效液相色谱分离和测定氨基酸：用N—羟基琥珀酰？…

以Ｎ－羟基琥珀酰亚胺－α－萘乙酸酯（ＳＩＮＡ）为氨基酸的柱前衍生试剂,反相高效液相色谱分离测定了１５种氨基酸。采用含１０ｍｍｏｌ／Ｌ ｐＨ５．０的乙酸－乙酸钠缓冲溶液的甲醇－乙酸乙酯－水（１０／２／８８,Ｖ／Ｖ／Ｖ）溶液为流动相体系。分离测定了７种氨基酸;用甲醇－乙酸乙酯－水（２６／２／７７,Ｖ／Ｖ／Ｖ）分离测定了５种氨基酸;用甲醇－乙酸乙酯－水（４５／２／５３,Ｖ／Ｖ／Ｖ）分离测定了３种氨基酸。     

方酸的合成进展

介绍了方酸（３,４－二羟基－３－环丁烯－１,２－二酮）的各种合成方法,评述了有机化学、电化学、生物发酵等方法合成方酸的进展及应用前景,参考文献２９篇。     

4’，5，7－三羟基－2’－甲氧基－6，8－二异戊烯基黄烷酮的全合成

以２，４，６－三羟基苯乙酮和间甲氧基苯酚为原料，分别经过异戊烯基化和保护羟基以及甲醛化，保护羟基，再通过缩合、环化、去甲氧基甲基等共七步反应，首次成功地合成了４’，５，７－三羟基－６，８－二异戊烯基黄烷酮。     

反相离子对高效液相色谱法分离和测定铝、镓和铟

以芪－４,４‘－双（１－偶氮）－３,４－二羟基苯－２,２’－二磺酸铵（芪唑）为柱前衍生试剂,采用反相离子对高效液相色谱法分离和测定铝,镓和铟。在ｓｐｈｅｒｅｘ Ｃ１８柱上,用浓度为１２ｍｍｏｌ／Ｌ的ＳＤＳ,浓度为２０ｍｍｏｌ／ｌ ｐＨ３．５的ＡＨｃ－ＮａＡｃ的甲醇－水溶液作流动相,检测波长为５０６ｎｍ。     

鳙鱼心中电子载体泛醌化合物的研究

鳙鱼（Ａｒｉｓｔｉｃｈｔｈｙｓｎｏｂｉｌｉｓ）心脏提取物经硅胶柱色谱分离、制备薄层色谱纯化，得到二种泛醌化合物，用ＮＭＲ、ＩＲ、ＭＳ、ＵＶ、ＨＰＬＣ、ＴＬＣ等现代测试技术测定其化学结构为２，３－二甲氧基－５－甲基－６－１０聚异戊二烯基－１，４－苯醌（Ⅰ）和一种未见报道的新泛醌酯——２，３－二甲氧基－５－甲基－６－甲酯基－八聚异戊二烯基－１，４－苯醌（Ⅱ）。     

3,4,5-三甲氧基苯甲酰腙类化合物的合成与表征

以没食子酸为原料。经烷基化、肼解得3,4,5-三甲氧基苯甲酰肼(2),2与芳香醛进行缩合反应合成了9个新的酰腙化合物。其结构经元素分析。IR,1H NMR和MS表征。     

3,4,5-三苄氧基苯甲酰腙类化合物的合成及生物活性研究

以没食子酸为起始原料,设计合成了10个新的3,4,5-三苄氧基苯甲酰腙类化合物4a~4j,其结构经元素分析、1HNMR和MS表征。初步的生物活性测试结果表明,所合成的化合物均表现出不同程度的抑菌活性,其中,4f的活性最好,在50 mg.L-1浓度下对水稻纹枯病菌和小麦赤霉病菌的抑制率达90%以上。     

2-氨基-4-氯-5-甲基苯磺酸的合成研究

2 氨基 4 氯 5 甲基苯磺酸是合成染料和颜料的重要中间体 ,主要用于合成Ｃ .Ｉ.颜料红等[1] 。目前该产品的合成是以对硝基甲苯为原料 ,经氯化、还原、磺化而成[2 ] 。磺化过程需在压力容器中进行 ,存在成本高 ,溶剂及副产物二氯苯、多氯联苯有毒等问题[3,4] 。为此采用无毒、价廉的汽油和石油醚作为混合溶剂 ,常压下合成 2 氨基 4 氯 5 甲基苯磺酸是本工作的目的。1　实验部分1 .1　主要仪器和药品Ｘ4熔点测定仪 ,日本 2 6 0 5 0型红外光谱仪 ,日本ＬＣ 6Ａ高效液相色谱仪 ,ＪＥＯＬＦＸ 90Ｑ型核磁共振光谱仪 ,美国ＰＥ 2 4 0 0自动元…     

The Synthesis and Reactions of N-Hydroxy-3-Arylsydnone-4-Carboxamide Oximes

N-Hydroxy-3-arylsydnone-4-carboxamide oximes (7) were prepared from the corresponding 3-arylsydnone-4-carbohydroximic acid chlorides (6) and hydroxylamine in high yield. The chemical reactivity of compound (2) is somewhat different from 3-arylsydnone-4-carboxamide oximes (2) in that the former compounds reacted with both aromatic and aliphatic aldehydes in the presence of acid catalyst to give 3-aryl-4-(5-aryl-1,2,4-oxadiazol-3-yl)sydnones (5) and 3-aryl-4-(5-alkyl-1,2,4-oxadiazol-3-yl)sydnones (3).     

Phosphor(V)-Hydrazin-Schwefel(IV)-Heterocyclen mit Twist-Boot-Konformation

Phosphorus(V)-Hydrazine-Sulfur(IV) Heterocycles with Twist-Boat Conformation . Unlike the corresponding unsubstituted compounds N-ethoxycarbonyl-substituted dihydrazidophosphoric acid derivatives do not react with thionylchloride under redoxdecomposition but yield sulfur containing sixmembered rings. In solution (NMR spectra) as well as in the crystal (X-ray structure analysis) the rings adopt unusual twist-boat conformations. Due to the rather bulky substituents high energies of interconversion between enantiomeric twist-forms are found: 75 ± 2 kJ/mol.     

The 1,3-Dipolar Cycloadditions of 3-Arylsydnone-4-Carbonitrile Oxides with Alkenes

3-Arylsydnone-4-carbonitrile oxides may undergo 1,3-dipolar cycloadditions with alkenes to produce the corresponding 3-aryl-4-(5-substituted-isoxazolin-3-yl)sydnones. The direct reaction of 3-arylsydone-4-carbohydroximic acid chlorides with alkenes may also give the same products, and with higher yield.     

Synthesis of 3-Aryl-4(3H)-quinazolinones from Anthranilic Acids and Triethyl Orthoformate

A one-step, convenient approach to the synthesis of 3-aryl-4(3H)-quinazolinones by the reaction of anthranilic acid with triethyl orthoformate in the presence of a catalytic amount of concentrated sulfuric acid has been developed. The possible reaction pathway was proposed.     

4-氧代-3（4H）-喹唑啉-5-羧酸的合成

以2-氨基-6-甲基苯甲酸为起始原料,通过合环反应生成两种4-氧代-3(4H)-喹唑啉-5-羧酸衍生物(1a, 1b), 1a, 1b分别经高锰酸钾氧化合成了4-氧代-3(4H)-喹唑啉-5-羧酸（2a, 2b）,其结构经¹H NMR, ¹³C NMR和MS表征。研究了投料比｛r［n(高锰酸钾) :n(5-甲基-3(4H)-喹唑啉-4-酮)］｝和反应温度等对收率的影响。结果表明：在最佳反应条件（r=7:1,中性高锰酸钾氧化,于90 ℃反应）下合成2总收率可达66%。     

Analysis of coptisine, berberine and palmatine in adulterated Chinese medicine by capillary electrophoresis-electrospray ion trap mass spectrometry

A rapid and simple reversed-phase liquid chromatographic method that did not require the derivatization of 4-amino-3-hydroxybutyric acid (GABOB) was developed and validated. The method proved to be suitable for the determination of GABOB concentrations in finished pharmaceutical product (tablets). The method was developed using a RP-18 column, UV detection at 210 nm and 0.01 M sodium heptasulphonate solution, at pH 2.4, as the mobile phase. Different validation parameters were included and satisfactorily evaluated. The specificity of the method was demonstrated. Linearity was established in the range 0.40–0.60 mg/ml (r=0.997). The method showed excellent accuracy (100.1%). Precision (repeatability) gave a relative standard deviation value of 0.68%, while the intermediate precision was 1.70%. A robustness test showing the influence of different pH values and counter-ion concentrations was also performed.     

Standard enthalpy of formation of 3,4,5-trimethoxybenzoic acid

The energy of combustion of crystalline 3,4,5-trimethoxybenzoic acid in oxygen at T=298.15 K was determined to be -4795.9±1.3 kJ mol^-1 using combustion calorimetry. The derived standard molar enthalpies of formation of 3,4,5-trimethoxybenzoic acid in crystalline and gaseous states at T=298.15 K, Δ_fH_m ^Θ (cr) and Δ_fH_m ^Θ (g), were -852.9±1.9 and -721.7±2.0 kJ mol^-1, respectively. The reliability of the results obtained was commented upon and compared with literature values. This revised version was published online in August 2006 with corrections to the Cover Date.