离子对高效液相色谱法分析注射用新灭菌

建立了离子对高效液相色谱法分离与测定复方制剂（新灭菌）中的羟氨苄青霉素及氟氯青霉素含量法。采用Ｃ８．１０μｍ，４．６×２００ｍｍ柱（大连化物所Ｓｐｈｅｒｉｓｏｒｂ），以含１．４％十六烷基三甲基溴化铵的ｐＨ６．５磷酸盐缓冲液－乙腈（６８＋３２）为流动相，在紫外检测器２５４ｎｍ波长处检测，线性范围为０．２５～２ｍｇ／ｍＬ，ｒ＝０．９９９９（ｎ＝５），羟氨苄青霉素及氟氯青霉素平均回收率分别为９９．５％及１００．７％（ｎ＝５）。精密度：羟氨苄青霉素及氟氯青霉素日内（４ｈ）平均ＲＳＤ（相对标准偏差）均为０．８％（ｎ＝１５），日间（２ｈ）平均ＲＳＤ分别为０．６％和０．７％（ｎ＝３）。     

阿斯美胶囊中四种组分的高效液相色谱分析

建立了反相高效液相色谱法测定阿斯美胶囊中氨茶碱、盐酸甲氧非那明、马来酸氯苯那敏及那可汀四种组分的含量。色谱柱为ＳｐｈｅｒｉｓｏｒｂＣ８，５μｍ，２００ｃｍ×４０ｍｍＩＤ，流动相为体积分数０５％的三乙胺溶液（磷酸调节ｐＨ５５）＋乙腈＋甲醇（５５０＋３６８＋８２），检测波长为２６４ｎｍ，线性范围分别为：氨茶碱３１２５～２５０ｍｇ／Ｌ，γ＝０９９９６，盐酸甲氧非那明１５６２５～１２５０ｍｇ／Ｌ，γ＝１００００，马来酸氯苯那敏２５～２００ｍｇ／Ｌ，γ＝０９９９９，那可汀８７５～７００ｍｇ／Ｌ，γ＝０９９９９；回收率（ｎ＝３）分别为１０１２％，１００８％，９９９％，９９５％；精密度：日内平均ＲＳＤ（ｎ＝６）分别为０７％，０４％，０４％，０６％；日间平均ＲＳＤ（ｎ＝３）分别为１０％，１０％，１１％，１２％。     

高效液相色谱法测定灭尔痛片的组分含量

采用高效液相色谱法同时测定灭尔痛片中对乙酰氨基酚、异丙基安替比林、及咖啡因３种成分的含量。色谱条件为：ＯＤＳ柱，甲醇＋水（６０＋４０）为流动相，检测波长为２５４ｎｍ。方法线性范围分别为：２４～１２０ｍｇ／Ｌ（ｒ＝０９９７６）；１２～６０ｍｇ／Ｌ（ｒ＝０９９９４）；４～２０ｍｇ／Ｌ（ｒ＝０９９９４）。各组分的平均回收率（ｎ＝６）分别为：１００３％，ＲＳＤ＝０４２％；９９７％，ＲＳＤ＝０６９％；９９２％，ＲＳＤ＝０４６％。该法操作简便、快捷，结果准确。     

柑桔皮精油中β—胡萝卜素,维生素E和硒含量的测定

柑桔皮精油用ＫＯＨ皂化，用无水乙醚提取不皂化物，蒸去乙醚，残渣用无水乙醇溶解，超滤后取清液注入高效液相色谱仪，以反相柱分离，紫外可见分光检测器检测其中的β－胡萝卜素和维生素Ｅ。柑桔皮精油用正丁醇适当稀释后直接用平台石墨炉原子吸收法测定其中的硒。测定结果：柑桔皮精油中β－胡萝卜素，维生素Ｅ和硒的含量分别为０１６８×１０－３（ＲＳＤ＝５４％，ｎ＝５），１８１×１０－３（ＲＳＤ＝７２％，ｎ＝５）和０５５×１０－６（ＲＳＤ＝３７％，ｎ＝９）。     

高效液相色谱法测定人血清中头孢克罗

建立了测定人血清中头孢克罗的高效液相色谱法。分析柱为Ｓｈｉｍ－ｐａｃｋＣＬＣ－ＯＤＳ（５μｍ）,６．０ｍｍ×１５０ｍｍ;流动相为磷酸盐缓冲液（ｐＨ５．８）∶乙腈＝８７．５∶１２．５,流速为１．２ｍＬ／ｍｉｎ;紫外检测波长为２５４ｎｍ。血清中头孢克罗浓度在０．１２５～２４ｍｇ／Ｌ范围内,峰高与浓度呈良好的线性关系,回归方程为Ｈ＝－３．２００＋９２．２９Ｃ（ｎ＝９,ｒ＝０．９９９９）,日内、日间变异系数分别为４．１％和５．８％,平均回收率为９９．３％。     

毛细管气相色谱法测定速效伤风胶囊中对乙酰氨基酚、咖啡因、马来酸氯苯那敏的含量

用５％Ｐｈ－Ｍｅ－Ｓｉｌｉｃｏｎｅ毛细管色谱柱，ＦＩＤ，二阶程序升温，以正十六烷作为内标物测定速效伤风胶囊中对乙酰氨基酚、咖啡因、马来酸氯苯那敏的含量。浓度线性范围：对乙酰氨基酚４～２０ｇ／Ｌ，咖啡因０．０８４～０．４２ｇ／Ｌ，马来酸氯苯那敏０．１５～０．７５ｇ／Ｌ。平均回收率（ｎ＝５）：对乙酰氨基酚９９．６２％（ＲＳＤ＝０．４４％）咖啡因９６．４６％（ＲＳＤ＝１．３２％），马来酸氯苯那敏９８．５５％（ＲＳＤ＝０．６５％）。     

毛细管气相色谱法测定速效伤风胶囊中对乙酰氨基酚、咖啡因、马来酸氯苯那敏的含量

 用５％Ｐｈ－Ｍｅ－Ｓｉｌｉｃｏｎｅ毛细管色谱柱，ＦＩＤ，二阶程序升温，以正十六烷作为内标物测定速效伤风胶囊中对乙酰氨基酚、咖啡因、马来酸氯苯那敏的含量。浓度线性范围：对乙酰氨基酚４～２０ｇ／Ｌ，咖啡因０．０８４～０．４２ｇ／Ｌ，马来酸氯苯那敏０．１５～０．７５ｇ／Ｌ。平均回收率（ｎ＝５）：对乙酰氨基酚９９．６２％（ＲＳＤ＝０．４４％）咖啡因９６．４６％（ＲＳＤ＝１．３２％），马来酸氯苯那敏９８．５５％（ＲＳＤ＝０．６５％）。     

羟肟酸法快速测定食用油主要营养必需脂肪酸

建立了用ＨＰＬＣ简便快速测定食用油主要营养必需脂肪酸的羟肟酸法。样品一步衍生成羟肟酸上机分析,不需分离纯化。线性范围为０．０５～０．６０ｇ／Ｌ,回收率９６．９３％,ＲＳＤ＝１．８０％（ｎ＝４）,日内和日间ＲＳＤ分别为１．２４％和１．６２％（ｎ＝６）。比较１８∶３,１８∶２和１８∶１的甲酯与相应的三脂肪酸甘油酯标准品衍生的标准曲线,发现二者转化率均相差近一倍,回收率实验和样品实测结果亦证实,选取甲酯标准品衍生作标准曲线用于油脂定量是不合理的。     

线性迭代法同时测定小儿退热灵片中乙酰水杨酸和苯巴比妥的含量

本文利用线性迭代法同时测定了小儿退热灵片中乙酰水扬酸和苯巴比妥的含量。乙酰水杨酸的回收率为９９．６％（ＲＳＤ＝０．５８％，ｎ＝６），苯巴比妥的回收率为１００．４％（ＲＳＤ＝１．６６％，ｎ＝６）。本法测定结果与黑龙江省药品标准方法测定结果基本一致，本法简单，快速，适合该剂剂中两组份的同时测定。     

多种维生素的高效液相色谱分离及应用

在ＳｐｈｅｒｉｓｏｒｂＣ１８柱上，采用含Ｌｉ２ＳＯ４－己烷磺酸钠－三乙胺的水溶液作流动相，同时分离测定四种水溶性维生素：Ｂ１、Ｂ２、Ｂ６及烟酰胺。四种化合物的回收率在９９．２％～９９．９％之间，ＲＳＤ为０．１６％～０．４９％（ｎ＝５）。方法应用于常见的复合维生素药物制剂的含量测定，结果满意。     

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%.     

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.     

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.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

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.