中文核心期刊 理化检验 化学分册

正《理化检验-化学分册》杂志在近年来开展专题报道的基础上,拟在2020年继续于第5,7,9期分别推出"药物分析"、"环境分析"和"矿物及金属材料分析"的专题报道,热忱欢迎相关领域的科研技术人员踊跃投稿。药物分析用药安全是关乎人类健康和民生的重要问题。本专题重点关注用于药物成品、临床药物、体内药物、保健品、中草药和中成药中营养成分、功效成分、药效成分、对人体有毒副作用的成分、激素类、违禁成分、添加剂等成分分析、结构确认、杂质检测等的新技术和新方法。本专题也关注毒品鉴别检验和食品中药物残留及毒素等组分的分析。环境分析环境分析是指采用适当的分析方法检测水环境、土壤环境以及空气环境中的物质,获得污染物监测数据、分析样品检测数据等环境数据,利用统计学方法分析环境数据之间的关系,发现环境污染的内在问题,从而为环境保护工作提供强有力的理论依据。本专题报道内容涉及水环境、土壤环境和空气环境等3大类环境中的物质分析,要求样品前处理方法新颖、分析方法先进、数据处理恰当,并且发现检测数据的内在规律,分析污染机理,合理评价环境污染现状,为解决实际环境问题提出合理的建设性建议。     

水环境中胞内外抗生素抗性基因分析的DNA提取方法及污染现状研究进展

新型污染物抗生素抗性基因(Antibiotic resistance genes,ARGs)对公共健康产生了严重威胁,其在水环境中的长期存在和传播引起了广泛重视。胞内与胞外ARGs在水环境中的分布规律和环境行为差异明显,对其污染状况进行研究有助于全面了解水环境中ARGs的传播特性。该文总结了5种常见水样微生物DNA提取方法及其在胞内和胞外ARGs检测研究中的应用状况,比较了污水系统、淡水系统及海水系统等典型水环境中胞内和胞外ARGs的污染状况和迁移传播特性。为进一步探究水环境中ARGs的分布特征与传播机制提供了技术手段及污染现状等基础信息,对控制ARGs在水环境中的传播扩散具有重要意义。     

理化检验化学分册 征稿启事2020专题报道

正中文核心期刊《理化检验-化学分册》杂志在近年来开展专题报道的基础上,拟在2020年继续于第5,7,9期分别推出"药物分析"、"环境分析"和"矿物及金属材料分析"的专题报道,热忱欢迎相关领域的科研技术人员踊跃投稿。·药物分析用药安全是关乎人类健康和民生的重要问题。本专题重点关注用于药物成品、临床药物、体内药物、保健品、中草药和中成药中营养成分、功效成分、药效成分、对人体有毒副作用的成分、激素类、违禁成分、添加剂等成分分析、结构确认、杂质检测等的新技术和新方法。本专题也关注毒品鉴别检验和食品中药物残留及毒素等组分的分析。·环境分析环境分析是指采用适当的分析方法检测水环境、土壤环境以及空气环境     

天然水体沉积物中有机氮的研究进展

对20多年来国际上关于沉积物中有机氮的研究做了综述和回顾。氮是重要的生源要素,是水环境中动植物新陈代谢不可或缺的元素之一,但过量易于造成生态环境巨大破坏,沉积物中有机氮与水体的交换可能会成为水体元素的“汇”和“源”。研究有机氮在沉积物水界面迁移转化过程是研究水环境的基础和关键,对氮元素的生态系统中的环境化学研究有十分重要的意义。     

标准物质在检测实验室质量控制中的应用

【】 本文介绍了检测中使用标准物质进行质量控制的重要意义,分别在盲样测试、期间核查和质量控制图应用方面提出了使用标准物质进行质量控制的三种方法,并通过在实验室获得的检测数据对上述应用方法作了实例说明,对检测实验室应用标准物质进行质量控制工作具有指导意义。     

文物材料原子光谱分析标准样品应用进展

原子光谱分析法在文物材料研究分析中应用广泛,由于该法属于相对分析法,需要使用相应标准样品对分析仪器进行校准以获得理想的分析结果,分析质量控制和数据质量评价也离不开标准样品,因此标准样品对于文物材料原子光谱分析具有重要意义。该文对文物材料原子光谱分析标准样品的分类及应用进展进行了综述,对未来该领域的发展提出了建议。     

抗生素不同解离形态在水环境中的光化学行为

表层水体中存在众多可解离的有机污染物,揭示其不同解离形态的环境光化学行为,对于污染物的环境持久性和风险评价具有重要意义.抗生素是在水环境中广泛存在的新型有机污染物,其中氟喹诺酮类(FQs)、磺胺类(SAs)、四环素类(TCs)等抗生素因分子结构中含有羧基、羟基和/或氨基等可电离基团,在水中以多种解离形态共存而备受关注.抗生素的多种解离形态不仅以不同的丰度共存于环境表层水体中,而且不同的解离形态表现出相异的环境光化学转化行为和风险.本文总结了水环境中可解离抗生素光化学行为研究的最新进展,介绍了pH值对直接和间接光解动力学的影响,着重评述了抗生素不同解离形态的光化学反应动力学、转化产物和路径,讨论了可解离抗生素光化学转化的环境半减期和风险,最后对抗生素不同解离形态的光化学行为研究进行了展望.     

对工业电池交流内阻测量的讨论(英文)

能源和环境的可持续发展是本世纪最重要的问题之一.二次电池是具有重要意义的高效储能器件,在电动汽车及混合动力汽车等实际应用中,经常会用到电池组,此时需要考虑电池组中每一个单体电池性能的一致性.内阻作为用于表征电池一致性的性能参数之一,对电池的工业制造和使用非常重要.目前,锂离子电池等二次电池的内阻测试都是按照国际电工委员会第61960号标准(2003)来进行的.本文从该标准的理论基础和其在内阻测试仪中的实际应用等方面出发,分析并指出了该测试标准中的问题,希望能为电池行业新标准的建立提供一定的指导,并有助于可持续能源设备及电动汽车用动力电池的开发.     

鸡肉中尼卡巴嗪残留基体标准样品的研制

为填补我国尼卡巴嗪药物残留基体标准样品的空白,建立了鸡肉中尼卡巴嗪残留基体标准样品的研制方法。通过在饲料中添加尼卡巴嗪药粉喂养白羽肉鸡,使药物在鸡体内自然代谢,得到尼卡巴嗪残留阳性动物。取鸡前胸肉制成肉糜,经均质、冷冻干燥、粉碎、筛分、包装、辐照灭菌等处理,制备了355份含有尼卡巴嗪残留的鸡肉冻干粉。按照国家标准样品的规范,进行了均匀性检验、稳定性检验、定值和不确定度分析。采用液相色谱-串联质谱法(LC-MS/MS)测定样品中的尼卡巴嗪含量,以8家具有资质的实验室进行协同定值。结果表明本批标准样品的均匀性和稳定性良好,在-70、4、25、50℃下能稳定保存14天,在-18℃下保存的稳定性可达12个月,符合国家标准样品的相关要求。最终确定标准样品中尼卡巴嗪的标准值为(157.7±11.0)μg·kg^-1(k=2)。该标准样品可用于尼卡巴嗪的检测方法优化、检测实验室的能力评价,对于食品中尼卡巴嗪残留检测具有重要意义。     

刚果红-溴化十六烷基吡啶光度法测定阴离子表面活性剂

日常生活中常用的表面活性剂多数是阴离子洗涤剂.洗涤剂进入水环境后,其分子聚集在水和其它介质的表面,产生泡沫、乳化和微粒悬浮等现象,隔绝水中氧与空气中氧的交换,影响水体净化,导致水质恶化,由此对水体的环境污染问题越来越严重,引起了人们的重视.因此, 准确快速地测定阴离子表面活性剂的含量, 对于研究其在环境中的转化、迁移及对生理过程的影响, 均具有重要意义.     

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.