香蕉型软糖中混合色素的一阶导数分光光度法测定

本文提出以一阶导数分光光度法测定香蕉型软糖中的混合色素。其中苹果绿在618和651nm处测量导数峰值之和,而柠檬黄则在175nm处减去苹果绿的干扰部份测量导数峰值之差。经实际样品分析验证获得了满意的结果,相对标准偏差为1.87％,回收率在95—100％之间。     

膜富集固相萃取-漫反射光谱法快速测定食品中柠檬黄北大核心CSCD

色素作为食品中常用的添加剂,近年来受到广泛关注。人工合成色素通常较天然色素色彩鲜艳、坚牢度大、稳定性强、价格低廉,所以有着广泛的应用[1]。柠檬黄是人工合成黄色素中具有代表性的一种,其为橙黄色均匀粉末,可溶于水,耐热性、耐光性等均好,被广泛用于饮料、固体食品中,但柠檬黄分子中含有苯环等结构,具有毒性,食品中最大使用量为100 mg·L-1[2]。因此,检测饮料中柠檬黄十分重要。     

膜富集固相萃取-漫反射光谱法快速测定食品中柠檬黄

正色素作为食品中常用的添加剂,近年来受到广泛关注。人工合成色素通常较天然色素色彩鲜艳、坚牢度大、稳定性强、价格低廉,所以有着广泛的应用~[1]。柠檬黄是人工合成黄色素中具有代表性的一种,其为橙黄色均匀粉末,可溶于水,耐热性、耐光性等均好,被广泛用于饮料、固体食品中,但柠檬黄分子中含有苯环等结构,具有毒性,食品中最大使用量为100 mg·L~(-1)~[2]。因此,检测饮料中柠檬黄十分重要。     

基于原子层沉积技术的壳层隔绝纳米粒子用于色素的增强拉曼光谱检测

以原子层沉积技术(ALD)制备出的壳层厚度为1 nm的Ag@Al_2O_3核壳纳米粒子为基底,采用壳层隔绝纳米粒子增强拉曼光谱(SHINERS)技术对色素检测进行探究。对Ag@Al_2O_3粒子的最佳粒径、色素检出限做了研究,并对实际样品中日落黄和柠檬黄的色素添加进行SHINERS检测。结果表明,对日落黄和柠檬黄具有最佳SHINERS效果的Ag@Al_2O_3粒子的最佳粒径为300 nm,方法对日落黄和柠檬黄标准溶液的检出限分别为10μg/L和100μg/L,对液体饮料中日落黄和柠檬黄标准品的SHINERS检出限分别为10 mg/L和50 mg/L,对所选实际样品中部分样品的日落黄和柠檬黄添加不符合国家标准。     

桔子粉中色素的导数分光光度法测定

桔子粉是用白砂糖、柠檬酸、香料以及色素加工而成的饮料。所用色素为柠檬黄和胭脂红。这两种由煤焦油产物提炼得到的人工合成色素具有毒性,用量太大时对人体健康不利。我国卫生规定这些人工合成色素的最大允许用量为万分之一。我们利用导数分光光度法不必进行预处理和解联立方程直接测定了桔子粉中色素的含量,相对标准偏差为±1.0％,平均回收率为97.3％。方法原理:从柠檬黄和胭脂红在Beckman DU-7HS型分光光度计上获得的—阶导数谱图。 (扫描速度为1200纳米/分,△λ为4.0)可知:在548nm处柠檬黄对胭脂红的谱图无干扰。为了求得柠檬在468nm处导数峰值,可以利用已知浓度的胭     

高效液相色谱法测定小米中柠檬黄含量

柠檬黄作为一种食用的合成色素,有使用方便、价格低廉、着色力强等优点,但食用过量会对人体造成伤害,国家卫生标准对此指标有明确的限量.但一些不法商贩为牟取暴利,以陈米为原料加入过量柠檬黄色素伪造新米,严重危害了消费者身体健康.     

导数吸附伏安法同时测定柠檬黄及日落黄

色素日落黄和柠檬黄在ｐＨ８．２的硼酸钠－酸介质中均有良好的吸附伏安波，但波峰相互重叠，难以同时测定。本文提出以二阶导数法对日落黄和柠檬黄的重叠伏安波谱进行分析，以达到日落黄和柠檬黄同时测定的目的，方法简便快速。本法分析几种饮料中的日落黄及柠檬黄，结果满意。     

表面等离子体共振生物传感器的构建及对柠檬黄的检测

建立了傅里叶-表面等离子体共振传感器(FT-surface plasmon resonance,FT-SPR)检测食品色素柠檬黄的方法。利用柠檬黄与柠檬黄小鼠单克隆抗体特异性结合的原理,将碳酰二亚胺盐酸盐法制备出的柠檬黄-牛血清白蛋白偶联物成功结合到传感器芯片上,通过溶液竞争法检测柠檬黄。建立了标准曲线,获得检出限13μg/L;研究了pH值对检测的影响,得到pH 7.4为适宜的体系酸度;回收实验、实际样品检测及干扰实验的结果表明,本方法对柠檬黄有高选择性。与紫外检测方法相比较,FT-SPR传感器检测柠檬黄方法表现出了选择性高和检出限低等优势。     

三种食用色素的电化学行为的理论计算与验证

用量子理论计算柠檬黄、日落黄、胭脂红的相对焓（Hm）、相对熵（Sm）,计算柠檬黄、日落黄、胭脂红的还原电位分别为-0．969,-0．901,-0．854V（vs．Ag／AgCl／Cl）。探讨了琼脂对色素的电催化机理,采用循环伏安法在玻碳琼脂电极上研究了食用色素柠檬黄、日落黄、胭脂红的电化学行为,分别于-1．064,-0．910,-0．882V（vs．Ag／AgCl／Cl）产生还原峰,理论预测与试验结果基本一致。     

迭代目标转换因子分析法在吸附伏安法中的应用──混合色素的同时测定

将迭代目标转换因子分析法应用于混合色素溶液吸附伏安波谱的解析,完成了苋菜红、日落黄、柠檬黄和胭脂红混合色素在磷酸氢二钠-柠檬酸缓冲溶液(pH=5.7)中的吸附伏安法同时测定,取得了较满意的结果。     

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.     

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.     

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.     

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.