浅谈酶标分析仪检定规程中存在的一些问题

酶标分析仪作为一种快速,灵敏度、准确度较高的测试分析仪器,广泛地应用于医疗卫生、检验检疫等行业。它的主要原理是依据酶与底物产生显色反应,不同物质有其各自的特征吸收谱线,并遵守朗伯-比耳定律。理论上某种物质若能与特定酶发生反应并能产生颜色均可用酶标分析仪进行定性     

荧光法酶标分析仪的校准方法

参考荧光法酶标分析仪的工作原理、出厂指标及相关标准，建立了荧光法酶标分析仪的校准方法。参考相关计量技术规范，对荧光法酶标仪的计量技术指标进行了研究，荧光法酶标分析仪的主要校准项目有检出限、测量线性、测量重复性。参考指标为线性相关系数不小于0.995，检出限不大于5×10^-10 g/mL，测量重复性不大于1.5%。利用校准案例对校准方法进行验证，结果表明建立的校准方法科学合理、可操作强，可为荧光法酶标分析仪的计量校准作参考。     

基质环境对氨基苯甲酸/硅凝胶复合材料荧光特性的影响

近年来，溶胶－凝胶技术在制备无机－有机复合材料中的应用越来越广泛犤１～６犦。该方法既可以制得具有很好机械性能和光学均匀性的块体材料，也可以制得薄膜和粉体材料。有机光学活性物质在无机基质中的存在状态及其化学环境，有机分子之间及有机分子与无机基质之间的相互作用对材料的热稳定性、光学特性以及实际应用影响极大犤７～１０犦。研究无机基质的微环境与有机光学活性分子之间的相互作用，对于复合材料的组成、性能、制备工艺的优化设计和实际应用至关重要。但是，目前有关这方面的系统研究报道很少。本文在硅溶胶中分别掺入了一…     

固体进样直接测定法测定铜精矿中汞

建立了固体进样直接测定法测定铜精矿中汞含量的方法。铜精矿样品在测汞仪的分解炉中经300℃干燥和750℃高温热分解后,汞被催化分解为汞原子,于850℃齐化成金汞齐。汞蒸气被氧气流带入单波长光学吸收池,在波长253.7 nm处测量汞的吸光度,采用标准曲线法计算汞量。方法的线性范围分别为0~1.00,0~100μg/mL,线性相关系数为0.9999,检出限分别为0.10,0.04 ng/g。5个汞含量不同的铜精矿样品测定结果的相对标准偏差为2.14%~4.35%(n=11),样品加标回收率为92.00%~104.02%。采用该方法分别对2个铜精矿样品和铜精矿国际标准物质进行测定,测定结果与标准分析方法测定值和标准物质标示值基本一致。该方法简便、快速、准确,可以作为标准方法推广使用。     

光学异构体拆分方法的进展

光学活性异构体物质广泛存在于自然界的生物体内,为生命起源的基本物质。蛋白质和酶等物质,就是由许多光学活性的氨基酸组成。     

邻氨基苯甲酸/SiO2复合材料制备及其光热特性

有机发光体以其较高的发光效率、快速响应能力和较宽的可调谐波长被广泛应用于光转换材料、非线性光学材料和激光材料[1-3]。但是有机物的光学性能不稳定和热稳定性较差,使其在许多方面的应用受到限制。为了提高其光学和热稳定性,常用的方法是将各种有机发光体掺杂在以正硅酸乙酯为原料制得的SiO2凝胶玻璃基质中[4-6]。SiO2凝胶通常采用溶胶 凝胶法通过水解缩合制备。制备时一般采用无机酸作催化剂在酸性条件下进行,对质子酸作用敏感的有机物在酸性条件下往往热稳定性、光学性能下降,甚至遭到破坏。本文以廉价水玻璃为原料,在潜伏酸的…     

酶标分析仪检定用中性滤光片的校准

提出酶标分析仪检定用中性滤光片的校准方法，并用校准实例对校准方法进行了验证。结合校准方法，根据JJF 1059.1—2012《测量不确定度评定与表示》建立了数学模型，不确定度的来源有测量结果的重复性、分光光度计透射比误差、分光光度计杂散辐射、中性滤光片年稳定性、中性滤光片均匀性，按该校准方法校准的中性滤光片，校准结果的不确定度为U=0.005(k=2)，校准结果能够满足JJG 861—2007《酶标分析仪检定规程》对中性滤光片不确定度U≤0.01(k=2)的要求，可用于开展酶标分析仪吸光度值的校准工作。     

紫外可见分光光度法测定酶解桑葚酒中多糖含量

采用紫外可见分光光度法测定酶解桑葚酒中的多糖含量。向酶解桑葚酒中加入硫酸,使样品中的多糖水解成单糖,并迅速脱水生成糖醛衍生物,加入苯酚作为显色剂,检测波长为490 nm,标准工作曲线线性方程为y=0.056 8x–0.035,相关系数r=0.999 4。测定结果的相对标准偏差为0.03%(n=5),平均加标回收率为98.69%。该方法用于检测酶解桑葚酒中多糖含量,简便、快速。     

奥科公司有志成为更专业更高效的标准物质供应商

<正>北京世纪奥科生物技术有限公司成立于2007年11月,于同年创建国家标准物质网站,依托该网站平台,专业从事标准物质产品销售和技术服务,是国内较大的标准物质提供商之一。国家标准物质网http://www.bzwz.com(bzwz)是国内一站式标准物质采购平台,汇集各类标准物质数10万种,涵盖各类国家标准物质、进口标准品、冶金标准样品、药品对照品、标     

用温度敏感高分子为载体的激光光声免疫分析及其应用

将单克隆抗乙肝表面抗原体抗与温度敏感高分子聚Ｎ－异丙基丙烯酰胺连接，中液相中与抗原、酶标抗体反应，通过热沉淀实现与游离酶标体抗体的异相分离。高分子载休的引入能减少非特异性吸附，罗大相载体聚乙烯酶标板更有利于激光光声技术高灵敏度优势的。同时，采用０．５％的十二烷基硫酸钠水溶液作显色终止剂，易与Ｈｅ－Ｎｅ激光波长匹配，实现了对低值乙肝表面抗原阳性血清的检测。     

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.