A sensitive DNA biosensor based on a facile sulfamide coupling reaction for capture probe immobilization

A novel DNA biosensor was fabricated through a facile sulfamide coupling reaction. First, the versatile sulfonic dye molecule of 1-amino-2-naphthol-4-sulfonate (AN-SO₃⁻) was electrodeposited on the surface of a glassy carbon electrode (GCE) to form a steady and ordered AN-SO₃⁻ layer. Then the amino-terminated capture probe was covalently grafted to the surface of SO₃⁻-AN deposited GCE through the sulfamide coupling reaction between the amino groups in the probe DNA and the sulfonic groups in the AN-SO₃⁻. The step-by-step modification process was characterized by electrochemistry and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy. Using Ru(NH₃)₆³⁺ as probe, the probe density and the hybridization efficiency of the biosensor were determined to be 3.18 × 10¹³ strands cm⁻² and 86.5%, respectively. The hybridization performance of the biosensor was examined by differential pulse voltammetry using Co(phen)₃^3+/2+ (phen = 1,10-phenanthroline) as the indicator. The selectivity experiments showed that the biosensor presented distinguishable response after hybridization with the three-base mismatched, non-complementary and complementary sequences. Under the optimal conditions, the oxidation peak currents of Co(phen)₃^3+/2+ increased linearly with the logarithm values of the concentration of the complementary sequences in the range from 1.0 × 10⁻¹³ M to 1.0 × 10⁻⁸ M with a regression coefficient of 0.9961. The detection limit was estimated to be 7.2 × 10⁻¹⁴ M based on 3σ.     

Ultra high performance liquid chromatography-quadrupole-time of flight analysis for the identification and the determination of resveratrol and its metabolites in mouse plasma

Resveratrol is a polyphenol that has numerous interesting biological properties, but, per os, it is quickly metabolized. Some of its metabolites are more concentrated than resveratrol, may have greater biological activities, and may act as a kind of store for resveratrol. Thus, to understand the biological impact of resveratrol on a physiological system, it is crucial to simultaneously analyze resveratrol and its metabolites in plasma. This study presents an analytical method based on UHPLC-Q-TOF mass spectrometry for the quantification of resveratrol and of its most common hydrophilic metabolites. The use of ¹³C- and D-labeled standards specific to each molecule led to a linear calibration curve on a larger concentration range than described previously. The use of high resolution mass spectrometry in the full scan mode enabled simultaneous identification and quantification of some hydrophilic metabolites not previously described in mice. In addition, UHPLC separation, allowing run times lower than 10 min, can be used in studies that requiring analysis of many samples.     

Synthesize,Characterization and Application of Phosphine‐free Polymer Supported Palladium Nanoparticles as Effective Catalyst in Suzuki‐Miyaura Cross‐coupling Reactions

Heterogeneous catalysts were developed by supporting palladium nanoparticles on modified cross‐linked polyacrylamide and successfully applied in Suzuki‐Miyaura cross‐coupling reactions. These catalysts are stable to air and moisture, and no sign of metal leaching was detected during the reactions as judged by elemental analysis of palladium by ICP‐OES technique and hot filtration test, which demonstrates the heterogeneous character of the catalysts. High yields of desired products were resulted by using these phosphine‐free catalysts at temperatures below 80 °C without aid of any additional ligands. The heat stability of the catalysts at the operating temperature was confirmed by thermogravimetric analysis (TGA). These catalysts are easy to use and cost effective. They can be recovered from reaction mixture by a simple filtration and reused in more successive reactions without significant loss in activity. The catalyst activity was restored by an ultrasonication program after deactivation in 10 cycles.     

Highly selective synthesis of novel (E)-styrylsilatranes via ruthenium-catalyzed trans-silylation

Protocols for the synthesis of cage-substituted 1-vinylsilatranes have been developed and updated. The 1-vinylsilatranes with organic substituents attached to silatrane cage were functionalized in ruthenium-catalyzed trans-silylation with olefins, leading to novel styrylsilatranes in high yields.     

Stereoselective Synthesis of Difunctionalized 1,3-Dienes Containing Silicon and Selenium via Hydrozirconation of (Z)-3-(Trimethylsilyl)alk-3-en-1-ynes

Sonogashira coupling of (E)-α-iodovinylsilanes 1 with (trimethylsilyl)-acetylene gave (Z)-1,3-bis(trimethylsilyl)alk-3-en-1-ynes 2, which underwent a desilylation reaction to afford (Z)-3-(trimethylsilyl)alk-3-en-1-ynes 3 in good yields. (1E,3Z)-1-Arylseleno-3-(trimethylsilyl)-substituted 1,3-dienes 5 could be synthesized stereoselectively via hydrozirconation of (Z)-3-(trimethylsilyl)alk-3-en-1-ynes 3, followed by trapping with arylselenenyl bromides.     

One‐Pot Synthetic Procedure for2,2′‐Disubstituted Biaryls via the Suzuki Coupling Reaction of Aryl Triflates in a Biphasic Solvent System

A one‐pot synthetic procedure for 2,2′‐disubstituted biaryls was developed via a Suzuki cross‐coupling reaction of aryl triflates in a biphasic solvent system. The effects of various bases and solvents were investigated. Results showed that the Na₂CO₃–toluene/H₂O combination gave the highest yields.     

L ‐Proline‐Promoted CuI‐Catalyzed C‐S Bond Formation between Aryl Iodides and Thiols

An improved, mild procedure for the CuI‐catalyzed coupling reactions of aryl iodides with aliphatic and aromatic thiols, using L ‐proline as the ligand, is reported. This procedure is noteworthy given its high generality and exceptional level of functional group toleration.     

Synthesis and Spectral Studies of Some Novel 2,5,9,10-Tetrahydro [7,8-g]benzo-8-arylpyrazolo[4,5-e][1,5-b]benzoxazonine via Phase Transfer Catalysis

Treatment of 1H-4,5-dihydro-3-aryl-5-(2-hydroxyaryl)pyrazole with o-dibromoxylene under liquid-liquid phase transfer catalytic conditions using tetra-n-butylammonium hydrogen sulphate or [18]-crown-6 as PT catalyst, benzene/chloroform as organic phase and 50% aqueous potassium hydroxide as second phase, afforded novel 2,5,9,10-tetrahydro [7,8-g] benzo-8-arylpyrazolo[4,5-e] [1,5-b] benzoxazonines.     

Highly meso-Diastereoselective Pinacol Coupling of Aromatic Aldehydes Mediated by Al Powder/Copper Sulfate in Water

Pinacol-type coupling reaction products presenting a high meso-diastereoselectivity (the ratio dl/meso was 4/96 up to 1/99) were obtained in fair to good yields (24–69%) using several aromatic aldehydes as starting materials and aluminium powder/copper sulfate as catalysts, in water, under reflux conditions.     

Immobilization of Pd Catalysts on Mesoporous Silica for Amine- and Copper-Free Sonogashira Coupling Reactions

Immobilization of catalysts on solid supports is a promising approach to combine the advantages of heterogeneous and homogeneous catalysts. Pd(PPh₃)₂Cl₂, known as an extremely active homogeneous catalyst for the Sonogashira coupling reaction, has been immobilized on high-surface-area MCF (mesocellular foams)–type mesoporous silica powder modified with 3-aminopropyltriethoxysilane and subsequently with diphenylphosphine. The functionalized MCF-type silica and supported catalysts have been characterized by x-ray photoelectron spectroscopy (XPS), fourier transform infrared spectroscopy (FTIR), elemental analysis, nitrogen sorption porosimetry, and scanning electron microscopy (SEM). Such supported Pd catalysts have proven to be useful recyclable reagents for copper- and amine-free Sonogashira coupling reactions of haloaromatic compounds with terminal alkynes.