甲苯二异氰酸酯交联氧化β-环糊精及其与透析膜复合吸附剂对尿素的吸附

由甲苯二异氰酸酯交联氧化β-环糊精与透析膜复合制得复合吸附剂，对尿素的吸附结果表明，复合吸附剂的透析膜既可有效地阻止人血清白蛋白与吸附剂接触，又可使尿素分子迅速透过膜而被吸附剂吸附，复合吸附剂能从人血清蛋白溶液中高选择性地吸附尿素，吸附量也有明显提高，由未复合时的10mg／g增至38mg／g．     

交联聚丙烯酰胺负载的氧化β—环糊精的合成及其对尿素的吸附性能

以交联聚丙烯酰胺为载体，合成了高分子负载的氧化β—环糊精，并研究了它在不同条件下对尿素分子的吸附性能。结果表明交联聚丙烯酸胺负载的氧化β—环糊精对尿素具有良好的吸附效果，最大吸附容量可达到９６．８ｍｇ／ｇ（尿素浓度为１３０ｍｇ／ｄＬ，ｐＨ＝７．４，０．０１Ｍ磷酸盐缓冲液，吸附温度３７℃）。     

NAK-12树脂脱除蚕蛹复合氨基酸异味及褐变物质的研究

本文研究了用NAK－12吸附树脂脱除蚕蛹复合氨基酸异味及褐变色素的条件，初步分析了蚕蛹复合氨基酸异味产生的原因，实验结果表明：当流速为3BV／h时，1ml NAK-12吸附树脂能吸附1．75g蚕蛹复合氨基酸中的异味物质；能吸附1．45g蚕蛹复合氨基酸中的褐变物质。甲醇是异味物质和褐变物质的良好洗脱剂，用pH1．0的甲醇以1BV／h流速洗脱，仅用3．5BV的洗脱剂即可完全洗脱异味物质和褐变物质，蚕蛹复合氨基酸异味产生的可能机理是：加热蚕蛹复合氨基酸液时，其苯丙氨酸，蛋氨酸，蛋氨酸，异亮氨酸，亮氨酸，苏氨酸被氧化脱氨，生成挥发性醛，而其褐变则是赖氨酸，精氨酸与还原糖发生Maillard反应生成褐变物质引起的。     

固体表面荧光法测定吸附于白骨壤和木榄叶片上的葸

以新鲜白骨壤和木榄叶片为基质,建立了直接测定吸附于叶片表面蒽（An）的固体表面荧光分析法（SSF）。考察了白骨壤和木榄叶片上An的吸附量随An暴露浓度、暴露时间等因素的变化情况。方法测定吸附于白骨壤叶片上An的线性范围为0．92～8．71μg/g,检出限为5．77ng/g,加标回收率为79．2％～85．9％;测定吸附于木榄叶片上An的线性范围为89．5～698．2ng／g,检出限为1．79ng/g,加标回收率为75．1％～102．3％;对于两种叶片,方法的相对标准偏差都小于10％。     

聚偏氟乙烯中空纤维亲和膜分离γ—球蛋白的研究（I）——聚偏氟乙烯中空纤维亲和膜的制备及其吸附性能

对聚偏氟乙烯(PVDF)中空纤维膜进行表面亲水化处理，再经活化、偶联制得了带有苯丙氨酸(Phe)的PVDF中空纤维亲和膜。制备过程中以光电子能谱(XPS)及红外光谱分析膜表面基团的变化，经亲水化处理及活化偶联后，膜表面的O和N含量分别从5．6％和0.6％增加到16．5％和3．0％，而F含量由38．3％降低为23．0％。将该亲和膜用于室温下血浆中γ—球蛋白的分离实验，在pH＝7．4，离子强度I＝0.18的缓冲液体系及进料质量浓度为1．0mg／mL条件下，该亲和膜对γ—球蛋白的吸附量可达到5．85mg／g膜；与市售γ-球蛋白相比，血浆中提取纯度可达83.9%。     

大孔吸附树脂提取麦拓莱霉素的工艺研究

研究了用大孔吸附树脂从发酵液中分离提取新型大环内酯类抗生素-麦拓莱霉素的吸附工艺过程，对吸附条件进行了优化，得到了适宜的操作条件．结果表明：NKA树脂为最佳吸附剂：吸附最佳pH值为10．32；吸附流速选择为1ml／min；NaCl的加入对吸附不利，选择NaCl浓度为0．6％左右，本实验条件下，发酵液中的麦拓莱霉素浓度为0．18mg／ml；NKA的吸附量可达33．7mg／g树脂。     

交联聚丙烯酸固载化氧化β-环糊精的合成及其对尿素的吸附性能

大孔交联聚丙烯酸树脂(D151和D152)用氯化亚砜转化为酰氯后,通过成酯反应固载β-环糊精,再进一步用高碘酸钠氧化,合成出具有环状多醛结构的交联聚丙烯酸固载化氧化β-环糊精。系统研究了反应条件对β-环糊精固载化反应的影响,发现摩尔投料比(—COC1/β-CD)为1.5—1/1、温度80℃、时间24 h为最佳固载反应条件。探讨交联聚丙烯酸固载化氧化β-环糊精对尿素的吸附性能,阐明了吸附时间、溶液中尿素浓度、及介质pH值等对吸附量的影响。在尿素浓度130 mg/dL、吸附时间4h、介质pH 7、温度25℃时,交联聚丙烯酸固载化氧化β-环糊精对尿素呈现出最大吸附量82.13 mg/g。     

反相高效液相色谱／质谱法同时测定鸡肉中5种喹诺酮药物残留

采用反相高效液相色谱／四级杆串联质谱（RP-HPLC／MS／MS）同时测定鸡肉中的5种喹诺酮药物（quinolones，QNs）。均质后的鸡肉样品采用磷酸盐缓冲溶液和乙腈的混和溶液提取。提取液经正己烷液-液分配（LLP）去除脂肪后，用C18固相萃取（SPE）柱净化，氨化甲醇洗脱，洗脱液用氮气吹干，流动相定容后，分析物采用LC／MS／MS电喷雾电离（ESI），正离子，多反应监测（MRM）模式检测，外标法定量。在添加浓度2．5～10μg/kg范围内，5种QNs的回收率在79．8％～95．1％之间；相对标准偏差（RSD）均小于11．7％。环丙沙星、丹诺沙星、恩诺沙星检出限（LOD）为0．5μg／kg，沙托沙星为1．0μg／kg，氟甲喹为0．1μg／kg。     

高效液相色谱法测定鸡蛋中呋喃唑酮的残留量

采用基体固相扩散和固相萃取相结合的技术,对鸡蛋中呋喃唑酮残留进行了提取和净化处理,建立了高效液相色谱法检测鸡蛋中呋喃唑酮残留量的方法。对呋喃唑酮在C18固定相和硅胶固相萃取柱上的保留行为进行了研究。采用液相色谱分离,外标法定量,呋喃唑酮标准溶液的峰面积与样品浓度在5μg／L～2．5mg／L范围内呈良好的线性关系,线性回归系数大于0．9999。鸡蛋样品中呋喃唑酮不同加入量的平均回收率在80．2％～91．1％;相对标准偏差在2．0％～9．5％;最低检出限为10μg／kg。分析方法具有良好的重现性．批内、批间定量结果的相对标准偏差均小于10％。     

用双（2，4，4－三甲基戊基）膦酸－Span80－甲苯乳状液膜迁移、分离稀土离子的研究

用双（２，４，４－三甲基戊基）膦酸－Ｓｐａｎ８０－甲苯乳状液膜研究了稀土离子的迁移行为。当膜相含１０ｘ１０￣（－３）～３．０ｘ１０￣（－３）ｍｏｌ／Ｌ双（２，４，４－三甲基戊基）膦酸和２％～４％（Ｗ／Ｖ）Ｓｐａｎ８０，内相含０．５０～２．０ｍｏｌ／ＬＨＣｌ，外相的ｐＨ为３．５～５０时，所有稀土离子都能快速并完全迁移。根据各稀土离子在此乳状液膜体系中迁移性质的差别，控制外相酸度，试验了稀土离子相互之间的分离情况。试验表明，用此乳状液膜体系分离稀土离子有良好的应用前景．     

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.