Recognition of α-Amino Acid from β- and γ-Amino Acid by N -Phosphorylation

The reactivity of N -phosphoryl f -alanine differs from N -phosphoryl g -alanine and N -phosphoryl n -amino butyric acid enormously. N -phospho- f -alanine could self-activate to yield N -phosphopeptides either in aqueous or nonaqueous media, but not g - or n -amino acid analogues. The mechanism of the reaction is discussed.     

A Novel Synthesis of 2-Alkylthiobenzothiazoles and 2-Alkylthiobenzoxazoles

Abstract

3H-Benzothiazole-2-thione and 3H-benzoxazole-2-thione were selectively S-alkylated by use of O-alkylisoureas as the alkylating reagents. The reactions could be performed under mild reaction conditions in short reaction times, and high yields were obtained using O-primary-alkylisoureas, whereas low yields were obtained with sec- and tert-alkylisoureas.     

Effect of Mineral Salts on Steady Rheological Properties of Nonionic Hydrophobically Modified Polyacrylamide and Its Stress-Relaxation Behavior

A micelle-forming polymerizable surfactant monomer, octylphenol polyoxyethylene acrylate (OP-10-AC), was synthesized, and then OP-10-AC was copolymerized with acrylamide (AM) to form nonionic hydrophobically modified polyacrylamide P(AM/OP-10-AC) through micellar copolymerization. In the absence of surfactants, it was investigated in detail that the effect of mineral salts and temperature on steady rheological properties of P(AM/OP-10-AC) solutions and the effect of concentrations on reduced viscosity of P(AM/OP-10-AC) in a dilute solution. The results indicate that concentrations of the copolymer, mineral salts and temperature had a strong influence on shear viscosity of P(AM/OP-10-AC) solutions, and the trend of reduced viscosity of P(AM/OP-10-AC) solutions was distinctly different from polyacrylamide with increasing concentrations of testing solutions. In addition, it was also investigated that stress-relaxation behavior of an aqueous solution of P(AM/OP-10-AC)/KCl. As a result, a stress-relaxation model of the copolymer solutions was proposed, which can further verify the correctness of the conclusion on stress-relaxation behavior of hydrophobic association hydrogels in the paper reported previously.     

pH-Responsive Nanocomposites From Methylcellulose and Attapulgite Nanorods: Synthesis,Swelling and Absorption Performance on Heavy Metal Ions

A pH-responsive methylcellulose-g-poly(sodium acrylate)/attapulgite (MC-g-PNaA/APT) nanocomposite superabsorbent was prepared by the free-radical solution polymerization of methylcellulose (MC), sodium acrylate (NaA) and nanoscale attapulgite (APT) in the presence of the crosslinker N,N′-methylene-bis-acrylamide (MBA). The structure and morphology of the nanocomposite were characterized by FTIR, FESEM, TEM, XRD and EDS techniques, and the effects of the amount of MBA, MC and APT nanorods on swelling behaviors were also evaluated. Results indicate that NaA has been grafted onto MC macromolecular chains and APT nanorods participated in polymerization by its active silanol groups, and APT led to a better dispersion in the MC-g-PNaA matrix. The incorporation of APT clearly enhanced the swelling capacity and rate of the superabsorbent. In addition, the nanocomposite exhibited excellent absorption capacity on heavy metal ions, and its absorption amounts on Ni²⁺, Cu²⁺ and Zn²⁺ ions reached 9.86, 7.66 and 21.86 times greater than active carbon (AC). The biopolymer-based nanocomposite superabsorbents can be used as a potential water-saving material and candidate of AC for heavy metal ion absorption.     

Preparation of Epoxy-Functionalized Magnetic Polymer Nanospheres for Magnetically Targeted Radiotherapy

Magnetic poly(styrene?methyl methacrylate-glycidyl methacrylate)/Fe₃O₄ nanospheres with epoxy groups were prepared by modified one-step mini-emulsion polymerization in the presence of Fe₃O₄ ferrofluids. The products were characterized by fourier-transform infrared spectrum, transmission electron microscopy, thermogravimetric analysis and vibrating sample magnetometer. After surface modification with diaminopropane, histidine was covalently linked to the amine group of magentic nanospheres using glutaraldehyde as crosslinker. Finally, the preliminary labeling study based on non-radioactive rhenium was carried out and the labeling efficiency reached 80.4%. Such magnetic nanospheres had promising potential in magnetically targeted radiotherapy of cancer.     

A Novel Fission Process in Mini-emulsion RAFT Polymerization: Shell Crosslinked Nanoparticles as a Model

Shell crosslinked nanoparticles, prepared from copolymerization of styrene and disulfide crosslinker, using poly(2-(dimethylamino)ethyl methacrylate) (PDMAEMA) as stabilizer and macroinitiator, exhibited a special fission behavior during the mini-emulsion RAFT polymerization process.     

Synthesis and Properties of Poly(Aryl Ether Ketone) Copolymers with Trifluoromethyl‐Substituted Benzene in the Side Chain

The new monomer (4‐(4′‐trifluoromethyl)phenoxyphenyl)hydroquinone (TFPOPH) was synthesized in a three‐step synthesis. A series of poly(aryl ether ketone) copolymers were prepared by the reaction of (4‐(4′‐Trifluoromethyl)phenoxyphenyl)hydroquinone and hydroquinone (HQ) with 4,4′‐difluorobenzophenone (DFB) in the presence of potassium carbonate in tretramethylene sulfone (TMS). Thermal analyses of the fluorinated copolymers showed that the glass transition temperature and 5.0% weight loss temperature are similar with that of PEEK, and the crystallinity decreased with increasing of TFPOPH. For the copolymer synthesized with the molar fraction of TFPOPH in the diphenol monomers (TFPOPH, HQ) being over 0.2, no cold crystallization temperature and melting temperature were detected, indicating that these copolymers are almost amorphous. The crystal structure of the copolymers with the molar fraction of TFPOPH being not higher than 0.2 is rhombic. The solubility in polar aprotic solvents of poly(aryl ether ketone)s copolymers increases and dielectric constant decreases step by step.     

Synthesis of Sub-100 nm Nanoparticles by Emulsifier-free Emulsion Polymerization of α-Methylstyrene,Methyl Methacrylate and Acrylic Acid

The emulsifier-free emulsion copolymerization of α-methylstyrene (AMS) and methyl methacrylate (MMA) in the presence of functional monomer acrylic acid (AA) was carried out in batch process, giving birth to sub-100 nm nanoparticles. The kinetics of polymerization was investigated. The morphology and size of particles were monitored by TEM. The influences of the functional monomer AA concentration, initiator ammonium persulfate (APS) concentration, and polymerization temperature were studied. It was found that AMS caused a drastic decrease in both the rate of polymerization and the average degree of polymerization. The activation energy calculated from Arrhenius plot turned out to be 83.6 kJ/mol.     

Simultaneous determination of thirteen main components and identification of eight major metabolites in Xuebijing Injection by UPLC/Q-TOF

An ultra performance liquid chromatographic method was used for the simultaneous identification and quantification of thirteen main components in Xuebijing Injection, including uridine, gallic acid, guanosine, danshensu, protocatechualdehyde, oxypaeoniflorin, hydroxysafflor yellow A, paeoniflorin, ferulic acid, safflor yellow A, senkyunolide I, senkyunolide H and salvianolic acid B. The chromatographic separation was performed on an Acquity UPLC BEH C₁₈ column (1.7-μm, 2.1 × 100 mm, i.d.) with a gradient elution of acetonitrile and 0.2% acetic acid at a flow rate of 0.4 mL/min. The method was validated for linearity (r ² > 0.9990), intra- and inter-day precision (RSD < 1.94%), accuracy (91.8–99.7%), recovery (96.8–103.8%), limits of detection (0.16–8.0 ng), and limits of quantification (0.54–26.8 ng). At least eight metabolites in prototype were found in rat plasma and urine after intravenous injection of 4 mL/kg doses of Xuebijing Injection. The proposed method could be utilized to qualify and control Xuebijing Injection to ensure its safety and efficacy in application.     

Synthesis, crystal structures, and properties of inorganic-organic hybrid complexes constructed from copper(II) macrocyclic fragment

Reaction of a macrocyclic copper(II) complex [Cu(L)](ClO₄)₂ · 3H₂O (I) (L = 1,3,10,12,16,19-hexaazatetracyclotetracosane) with a hexapod carboxylate ligand H₆TTHA (H₆TTHA = 1,3,5-triazine-2,4,6-triamine hexaacetic acid) and a tripod carboxylate ligand H₃TATB (H₃TATB = 4,4′,4″-S-triazine-2,4,6-triyl-tribenzoic acid) yielded two mononuclear copper(II) complexes [Cu(L)][H₄TTHA] · 4H₂O (II) and [Cu(L)][HTATB] · 4H₂O (III). The complexes I–III have been structurally characterized. The crystal structures of complexes II and III show the copper(II) ion has a distorted pentacoordinate square-pyramidal geometry with two secondary and two tertiary amines from the macrocyclic complex [Cu(L)]²⁺ and one oxygen atom from the carboxylate ligand group at the axial position. The UV-Vis spectra are utilized to discuss the hydrolysis of the complex II.