反相高效液相色谱检测丹参药材中4种丹参酮的含量

建立了测定丹参药材中4种丹参酮含量的反相高效液相色谱法，色谱条件：流动相为水(含0．5％三乙胺)-甲醇-四氢呋喃(45／55／5，V／V／V)，流速为1mL/min；PDA检测波长254m；4种成分丹参酮Ⅰ、丹参酮ⅡA、隐丹参酮和二氢丹参酮的加样回收率在95．1％-101．2％之间，线性范围为0．08-2μg。该方法准确，稳定，重现性好。根据该色谱条件，测定了不同产地的丹参药材，结果表明：该色谱方法准确检测了生药中4种丹参酮的含量，适合于丹参药材的质量控制。     

一种测定MDR肿瘤细胞内外阿霉素浓度的方法

研究提出K562／A细胞内外阿霉素浓度的反相高效液相色谱-荧光测定法．细胞内阿霉素浓度测定采用Lichrospher C18色谱柱,甲醇-0．01％醋酸(50：50,V／V)流动相,流速1．0mL／min,柱温35℃;细胞外阿霉素浓度测定采用Lichrospher C18色谱柱,甲醇-0．01％醋酸(55：45,V/V)流动相,流速0．8mL／min,柱温35℃．荧光检测器波长λex=495nm,λem=560nm,均以盐酸柔红霉素为内标．研究结果表明,该方法简单、准确、线性范围宽、检测限低,精确度和回收率良好,可用于多药耐药肿瘤细胞内外阿霉素浓度的动态变化规律研究．     

固相萃取富集-高效液相色谱法测定环境水中多菌灵和噻菌灵

建立了以固相萃取技术富集，高效液相色谱法进行分离和检测多菌灵和噻菌灵2种杀菌剂的方法。环境水中的多菌灵和噻菌灵用3M Empore 6mL C18 Cartridge进行固相萃取。以Hypersil ODS柱为分析柱，优化得到高效液相色谱分离条件：流动相为甲醇-水(50：50，V/V)；流速为0．7mL／min；柱温为55℃；在286nm波长下检测，检出限为0．05mg／L。本法操作简便，灵敏，回收率高。     

固相萃取富集-高效液相色谱法分离检测水中3种苯脲除草剂

建立了固相萃取富集-高效液相色谱分析水中3种痕量苯脲除草剂——利谷隆、敌草隆、灭草隆的方法。C18固相萃取柱富集水中待测组分,高效液相色谱以Hypersil ODS柱为分析柱,优化出的色谱条件为：流动相为甲醇／水=60：40(V／V);流速为0．7mL／min;柱温为30℃。本法操作简便、灵敏、回收率高。     

高效液相色谱法测定生姜中的6-姜酚

用C18色谱柱，以V(甲醇)：V(水)：V(冰乙酸)=35：64：1溶液作流动相，进样量5μL，在流速1．0mL／min下，可不经分离直接测定生姜中的6-姜酚。方法RSD小于1．00％，回收率97％～102％，相关系数0．9999。     

利用酰胺型手性固定相高效液相色谱法对格列美脲顺反异构体的分离与测定

利用高效液相色谱法在一种酰胺型手性固定相上直接分离了格列美脲顺反异构体。讨论了流动相组成、柱温度和流速等色谱条件对分离的影响。优化的实验条件为：流动相组成正己烷：1,2-二氯乙烷：甲醇(88：8：4,V/V/V);柱温：25℃;流速：1．8mL／min。得到的分离度和选择性因子分别为1．86和1．12。在2．88～320mg／L的浓度范围内建立了反式格列美脲的标准曲线,线性系数为0．99998;检出限为0．47mg/L。方法简单,可靠,可用于实际格列美脲产品的定量分析。     

高效液相色谱法测定珍菊降压片中氢氯噻嗪的含量

用高效液相色谱法测定珍菊降压片中氢氯噻嗪的含量。色谱柱为C18反相柱,流动相为甲醇-水溶液(甲醇与水的体积比为2：3),流速为0．5mL／min,检测波长为277nm。氢氯噻嗪的质量浓度在18．24～42．56μg/mL内与对应的色谱峰面积呈线性关系,测定结果的相对标准偏差为0．78％,氢氯噻嗪的回收率为99．93％。     

高效液相色谱法测定小鼠血浆和组织中的阿昔洛韦

改良HPLC用于测定小鼠血浆和组织中阿昔洛韦浓度。使用Beckinan Gold系列高效液相色谱仪,ODS柱,流动相为甲醇－水（5：95,V／V）,流速1．0mL/min,检测波长254nm,样品采用12％三氯醋酸去蛋白。血浆和组织中阿昔洛韦浓度在0．05－20mg/L范围内与峰高呈良好线性关系,最低检测浓度分别为0.02.0.05mg/L,天间精密度均优于6％。     

高效液相色谱法测定前列泰片中山萘素的含量

建立了测定中药复方制剂前列泰片中山萘素含量的高效液相色谱方法．采用Kromasil C18色谱柱（5μm,250mm×4．6mm）,以甲醇：0．1％磷酸溶液=62：38（V／V）为流动相,流速1．0mL／min,检测波长为366nm．对样品水解过程中各个影响因素进行了考察,获得优化的水解条件为采用4．5mol／L盐酸溶液,80℃水浴上水解1．5h．山萘素在0．061～610μg／mL范围内峰面积与浓度呈良好的线性关系（r为0．9999）,最低检出限为0．03μg／mL,平均加标回收率为95．4％,RSD为1．4％．该方法简便、准确、重现性好,可用于前列泰片的质量控制．     

高效液相色谱法分离与测定柴胡中的柴胡皂甙a

采用反相高效液相色谱法对北柴胡中的柴胡皂甙a进行了分离和测定。试验选出分离的最佳条件：流动相为V（乙腈）：V（水）=90：10,流速为0．8mL／min,检测波长为208nm,在0．05—1．50mg／mL范围内柴胡皂甙a的量与峰面积线性关系良好,回归方程为：Y=2258428p＋186676,相关系数r=0．9993,检出限为2．3ng／mL,回收率为98．3％-100．9％。     

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.