HPLC法快速测定峰皇浆及制品中添加的维生素B6

本文研究了快速、简便测定蜂皇浆及制品中添加的低含量维生素Ｂ_６的ＨＰＬＣ法。称取适量样品，用１０％偏磷酸提取、净化，清液供ＨＰＬＣ分析用。ＷＡＴＥＲＳ荧光检测器，激发波长２９０ｎｍ，发射波长３９０ｎｍ，ＶＢ_６含量在０～１２０ｎｇ之间工作曲线相关系数大于０．９９９，样品中ＶＢ_６含量为０．１％～５％时，方法回收率为９２．１７％～９８．４２％，相对标准偏差（ｎ＝６）小于３．７％。     

高效液相色谱法测定强化奶及食品中维生素D含量

介绍用反相高效液相色谱法（ＨＰＬＣ）测定食品中ＶＤ含量,样品经皂化、正己烷提取、正相ＨＰＬＣ净化,用反相ＨＰＬＣ定量分析。回收率为９４．８８％～９９．７０％,批内和批间ＣＶ分别为１．６２％和２．１２％。分析了奶粉、要素膳、肉松、儿保饮料等８种食品中ＶＤ含量,亦可用于各种食品中ＶＤ分析。     

高效液相色谱法和毛细管电泳法测定甘草制品中甘草酸的含量

分别用高效液相色谱法（ＨＰＬＣ）、毛细管区带电泳法（ＣＺＥ）、胶束电动毛细管色谱法（ＭＥＣＣ）测定了甘草制品中甘草酸的含量。对ＨＰＬＣ,ＣＺＥ,ＭＥＣＣ的分析条件作了一些选择实验,结果表明ＭＥＣＣ法与ＨＰＬＣ法分析数据接近、比较准确,而且前者比ＨＰＬＣ法分离效率高、溶剂用量少,是一种很有发展潜力的分析方法。     

蔗渣水解液及发酵液中糖及糖醇的高效液相色谱分析

采用ＨＰＬＣ测蔗渣水解液及发酵液中木糖、木糖醇等。在ＳｐｈｅｒｉｓｏｒｂＮＨ２柱上用乙腈＋水（８０＋２０）分离，示差折光检测器检测， １５ｍｉｎ内同时分离测定木糖、木糖醇及其它五种糖。线性范围在 ０～７．５ ｇ／Ｌ，相对偏差小于４．１％。     

高效液相色谱法测定利康冒胶囊中扑尔敏、扑热息痛、DL－盐酸甲基麻黄碱和咖啡因的含量

 介绍了用高效液相色谱法（ＨＰＬＣ）同时测定利康冒胶囊中扑尔敏、扑热息痛、ＤＬ－盐酸甲基麻黄碱和咖啡因的方法，色谱柱为ＲｅｓｏｌｖｅＣ（１８）柱，以乙腈：０．１％磷酸：三乙胺（８０：９１９：１）为流动相，检测波长２２０ｎｍ，柱温３５℃。各组分的平均回收率为９７％～９９％，日内测定的变异系数小于２％，是一种精密、灵敏的方法，可用于药品质量控制。     

高效液相色谱法测定利康冒胶囊中扑尔敏、扑热息痛、DL－盐酸甲基麻黄碱和咖啡因的含量

介绍了用高效液相色谱法（ＨＰＬＣ）同时测定利康冒胶囊中扑尔敏、扑热息痛、ＤＬ－盐酸甲基麻黄碱和咖啡因的方法，色谱柱为ＲｅｓｏｌｖｅＣ（１８）柱，以乙腈：０．１％磷酸：三乙胺（８０：９１９：１）为流动相，检测波长２２０ｎｍ，柱温３５℃。各组分的平均回收率为９７％～９９％，日内测定的变异系数小于２％，是一种精密、灵敏的方法，可用于药品质量控制。     

高效液相色谱和高效液相色谱—质谱法测定粮食中互隔交链孢霉醇,互隔交…

建立了粮食中互隔交链孢霉醇，互隔交链孢霉醇单甲醚和玉米赤烯酮三个毒素的ＨＰＬＣ定性定量分析法和粒子束ＬＣ－ＭＳ／ＥＩ＾＋鉴定方法，采用反相色谱，以８０％的甲醇水溶液作流动相，这三个毒素在Ｃ１８色谱柱上彼此间均获得较好的分离，方法对粮食中ＡＯＨ，ＡＭＥ两个毒素的回收率均在７９％以上，ＡＯＨ，ＡＭＥ两个毒素的最低检出限为１×１０＾－９ｇ。用所建立方法对１００多个大骨节病病区，非病区的粮食样品进行了检测     

钴铜锰镍的HPLC的研究及其在中草药微量元素形态分析中的应用

本在对Ｃｄ、Ｃｏ、Ｃｕ、Ｆｅ、Ｍｎ、Ｎｉ、Ｓｅ、Ｚｎ的二乙基二硫代氨基甲酸螯合物ＨＰＬＣ行为研究的基础上，提出了Ｃｏ、Ｃｕ、Ｍｎ、Ｎｉ的反相ＨＰＬＣ法，并用于中经中这些元素的初级形态分析。     

反相高效液相色谱分离—安培法检测酚类化合物

本文报道了ＲＰ－ＨＰＬＣ－安培法检测测定酚类化合物的条件，在Ｓｈｉｍ－ｐａｃｋＣＬＣ－Ｃ８柱上用含０．５ｍｏｌ／Ｌ ＮａＨ２ＰＯ４缓冲溶液的５％甲醇水溶液洗脱分离，于Ｅ＋１．０Ｖ处检测，线性范围在０－７μｇ／ｍｌ，检测限达ｎｇ／ｍｌ。     

HPLC检测柑桔类水果中无机溴化合物残留量

采用ＨＰＬＣＳｈｉｍ－ｐａｃｋＩＣ－Ａ１柱，紫外检测器测定柑桔类水果中无机溴残留量，样品经氢氧化钠乙醇溶液水解，灰化后进行ＨＰＬＣ分析。方法简便，重复性好（ＣＶ＝０．９５～８．６１％），样品检出限为１０￣（－６），添加回收大于９０％。     

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%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

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.     

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.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

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.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.