Monoolein cubic phase containing disulfide proteinoid and its reduction-responsive release property

Monoolein (MO) cubic phase, which can release its payload in answering to reducing condition, was prepared by including a disulfide proteinoid composed of Asp, DL-leucine (Leu), and dithiodipropionic acid (DTPA) in its water channel. On the TEM micrograph, the cubic phase could accommodate the proteinoid with no change in its bilayer structure. The phase transition temperature of the cubic phase was about 58.7°C, and it was little affected by the proteinoid. The release degree of allura red loaded in the cubic phase was higher at a higher dithiothreitol (DTT) concentration. The proteinoid would be broken down by the reducing agent, facilitating the release.     

Complex Reducing Agents (CRA's)—Versatile,Novel Ways of Using Sodium Hydride in Organic Synthesis

Why do we hardly use the simplest and, at the same time, inexpensive reducing agent sodium hydride in organic chemistry? To this question the answer is invariably: “It is too basic”. In this progress report we describe work we have performed aimed at controlling the basicity of NaH using sodium alcoholates and metal salts. The complex reducing agents (CRA's) developed (symbolized NaH-RONa-MX_n) allow organic halides, alkenes, alkynes and ketones to be reduced selectively. Highly regioselective 1,4- and 1,2-reductions of α,β-unsaturated ketones are easily performed using appropriate metal salts. Modified CRA's have proved to be excellent hydrosilylating reagents for carbonyl groups, non-pyrophoric heterogeneous hydrogenation catalysts, coupling reagents for aryl and vinyl halides, and reagents for the carbonylation of organic halides under very mild conditions. The study of these reactions opened up the field to phase-transfer-catalyzed photostimulated carbonylations as well as to S_RN1 reactions of metalates.–Thus, starting from the simple sodium hydride a large number of useful reagents have become accessible.     

Integrating approach to discover novel bergenin derivatives and phenolics with antioxidant and anti-inflammatory activities from bio-active fraction of Syzygium brachythyrsum

Syzygium brachythyrsum is an important folk medicinal and edible plant in Yunnan ethnic minority community of China, however, little is known about the chemical and bio-active properties. The present study is aimed to identify the bioactive constituents with antioxidant and anti-inflammatory properties by an integrating approach. First, two new bergenin derivatives, brachythol A (1) and brachythol B (2), together with eleven known phenolic compounds (3–13) were isolated from bioactive fractions by phytochemical method. Among these isolated chemicals, five bergenin derivatives, along with 3 phenolics were found in Syzygium genus for the first time. Then, a further chemical investigation based on ultra-high-performance liquid chromatography-Q Exactive Orbitrap mass spectrometry resulted in a total of 107 compounds characterized in the bio-active fractions, including 50 bergenin derivatives, among which 14 bergenin derivatives and 14 phenolics were potential new natural chemicals. Most of the isolated compounds showed obvious antioxidant activities, while compounds 11, 12, and 13 had favorable performance. Eight compounds (2–5, 7, and 9–11) showed good inhibitory activity on nitric oxide (NO) production in macrophage RAW 264.7 cells. The structure–activity correlation analysis indicated that the antioxidation and anti-inflammatory activities enhanced when bergenin was esterified with gallic acid, caffeic acid or ferulic acid. This is the first report of bergenins in Syzygium genus and the richness in new bio-active bergenins and gallic acid derivatives indicated that Syzygium brachythyrsum is a promising functional and medicinal resource.     

基于斐林试剂检测柿霜中还原糖含量的实验设计*

柿饼表面的柿霜主要成分是还原糖,基于斐林试剂与还原糖发生氧化还原反应的原理,可利用稀释定律对柿霜中还原糖含量进行测定。在定量滴定分析中,对斐林试剂的组成、滴定方式以及滴定计算方法进行了探究,并探讨了反应时溶液pH、斐林试剂用量和温度对实验的影响。与经典的碘量法比较,本方法的精密度和准确度都比较理想,是一种更为简便的还原糖含量测定方法。本实验有助于增强学生的食品安全意识,提高学生在滴定分析中数据处理的能力,可替代碘量法成为分析化学实验中一个新的实验。     

Chemical composition and antioxidant activity of aerial parts of Ferula longipes Coss. ex Bonnier and Maury

This is the first study on the phytochemistry and antioxidant activity of Ferula longipes Coss. ex Bonnier and Maury (Apiaceae). A new flavonoid quercetin-3-O-α-L-rhamnopyranoside-7-O-ß-D-[2-O-caffeoyl]-glucopyranoside (1), along with 10 known compounds kaempferol-3-O-α-L-rhamnopyranoside (2), quercetin-3-O-α-L-rhamnopyranoside (3), kaempferol-3-O-ß-D-glucopyranoside-7-O-α-L-rhamnopyranoside (4), isorhamnetin-3-O-α-L-rhamnopyranoside-7-O-ß-D-glucopyranoside (5), quercetin-3-O-α-L-rhamnopyranoside-7-O-ß-D-glucopyranoside (6), isorhamnetin-3,7-di-O-β-D-glucopyranoside (7), apigenin (8), apigenin-7-O-ß-D-glucopyranoside (9), 3,5-dicaffeoylquinic acid (10), deltoin (11) were isolated from the aerial parts of Ferula longipes Coss. Structures elucidation was performed by comprehensive 1D and 2D NMR analyses, mass spectrometry and by comparison with literature data. The compounds 1, 3, 4, 6, 7 and 10 were evaluated for their antioxidant activity, compound 1 exhibited the best antiradical activity potential and showed IC₅₀ and A_0.5 values 5.70, 7.25, 5.00, and 2.63 μg/mL towards DPPH free radical-scavenging, ABTS, CUPRAC, and reducing power assays, respectively compared with BHA, BHT and ascorbic acid which were used as positive controls.     

响应面法对3,5-二硝基水杨酸比色法测定水果中还原糖含量条件的优化

采用3,5-二硝基水杨酸(DNS)比色法测定水果中还原糖的含量,在单因素试验的基础上,采用三因素三水平的响应面分析法(RSM)优化DNS法测定苹果还原糖的最佳条件,同时建立数学模型并验证其可靠性。回归方程失拟项不显著(P=0.133 7),预测值与实际值吻合(R~2=0.957 4);影响DNS法测定还原糖含量的因素主次顺序为:DNS用量﹥反应温度﹥显色时间;DNS法测定还原糖含量的最佳条件为:DNS用量4.0 m L,显色时间5.0 min,反应温度87.0℃,测得还原糖实际浓度为94.66 mg/L,与理论预测值基本相符。按照优化的最佳条件,以苹果、桃、葡萄、哈密瓜、脐橙、菠萝6种代表性水果为对象验证该方法的精密度、重复性和准确度,其标准偏差为0.1%~0.5%,相对标准偏差为2.0%~4.8%,加标回收率为90.6%~104.2%。该方法简便、快速,准确度高,重现性好,适合于苹果及其他水果中还原糖的测定。     

常压下酸催化菊糖水解反应动力学研究

研究了菊芋中菊糖的酸催化水解。通过改变常压下菊糖酸催化水解的反应条件研究了反应动力学 ,得出该反应符合一级串连反应规律的结论     

Synthesis of 4-Aminopyrazol-5-ols as Edaravone Analogs and Their Antioxidant Activity

One of the powerful antioxidants used clinically is Edaravone (EDA). We synthesized a series of new EDA analogs, 4-aminopyrazol-5-ol hydrochlorides, including polyfluoroalkyl derivatives, via the reduction of 4-hydroxyiminopyrazol-5-ones. The primary antioxidant activity of the compounds in comparison with EDA was investigated in vitro using ABTS, FRAP, and ORAC tests. In all tests, 4-Amino-3-pyrazol-5-ols were effective. The lead compound, 4-amino-3-methyl-1-phenylpyrazol-5-ol hydrochloride (APH), showed the following activities: ABTS, 0.93 TEAC; FRAP, 0.98 TE; and ORAC, 4.39 TE. APH and its NH-analog were not cytotoxic against cultured normal human fibroblasts even at 100 μM, in contrast to EDA. According to QM calculations, 4-aminopyrazolols were characterized by lower gaps, IP, and η compared to 4-hydroxyiminopyrazol-5-ones, consistent with their higher antioxidant activities in ABTS and FRAP tests, realized by the SET mechanism. The radical-scavenging action evaluated in the ORAC test occurred by the HAT mechanism through OH bond breaking in all compounds, directly dependent on the dissociation energy of the OH bond. All the studied compounds demonstrated the absence of anticholinesterase activity and moderate inhibition of CES by some 4-aminopyrazolols. Thus, the lead compound APH was found to be a good antioxidant with the potential to be developed as a novel therapeutic drug candidate in the treatment of diseases associated with oxidative stress.     

NbSe2纳米材料的合成及减摩性能研究

将Se粉和Nb粉按一定的比例混合,然后密封在石英管中或压成片状后密封于石英管中,加热到一定温度,分别获得了NbSe2纳米纤维和NbSe2纳米颗粒.采用X射线衍射仪(XRD)、透射电子显微镜(TEM)和扫描电子显微镜(SEM)对所得产物进行了表征,分析了其微观形貌;采用MS-T3000摩擦磨损试验机测定了纳米颗粒作为基础润滑油N40添加剂的摩擦学性能.结果表明,制备的纳米纤维直径100～200nm,纳米颗粒直径40～300nm,二者都具有层状结构和良好的结晶性;NbSe2纳米颗粒作为润滑油添加剂具有明显优于基础润滑油的极压减摩性能;同纳米纤维相比,纳米颗粒的减摩性能较好.