[Design, synthesis and activity of N-acyl-thiochromenothiazol-2-amine as acetylcholinesterase inhibitors].

A series of novel N-acyl-thiochromenothiazol-2-amine derivatives were designed and synthesized, furthermore, their inhibition effect on acetylcholinesterase was investigated. N-Acyl-thiochromenothiazol-2-amines were prepared from thiophenol by Hantzsch reaction, acylation reaction and substitution reaction. Moreover, their bioactivities as AChE inhibitors in vitro were measured with Ellman spectrophotometry.

In situ polymerization of monolith based on poly(Triallyl Isocyanurate-co-trimethylolpropane triacrylate) and its application in high-performance liquid chromatography.

A novel organic monolithic stationary phase was prepared for high-performance liquid chromatography (HPLC) by in situ copolymerization. In which, triallyl isocyanurate (TAIC) and trimethylolpropane triacrylate (TMPTA) in a binary porogenic solvent consisting of polyethylene glycol 200 and 1, 2-propanediol were used. The resultant monoliths with different column properties (e.

[Design, synthesis and evaluation of N-acyl-4-phenylthiazole-2-amines as acetylcholinesterase inhibitors].

N-Acyl-4-phenylthiazole-2-amines were designed and synthesized, moreover their effects on acetylcholinesterase activities were tested. N-Acyl-4-phenylthiazole-2-amines were prepared from substituted 2-bromo-1-acetophenones by three steps reaction, and their AChE inhibitory activities were measured by Ellman method in vitro. The results showed that the target compounds had a certain inhibitory activity on AChE in vitro.

One-pot three-component synthesis of 3-hydroxy-5,5-dimethyl-2-[phenyl(phenylthio)methyl]cyclohex-2-enone derivatives under ultrasound.

3-Hydroxy-5,5-dimethyl-2-[phenyl(phenylthio)methyl]cyclohex-2-enone is synthesized via one-pot three-component reactions of aromatic aldehyde, substituted thiophenol and 5,5-dimethyl-1,3-cyclohexanedione catalyzed by p-dodecylbenzene sulfonic acid (DBSA) under ultrasound. Under ultrasound irradiation the yields are much higher (sometimes substantially, by almost double) and the reaction time decreases substantially, the reaction conditions are milder. This method provides several advantages such as environment friendliness, high yields and simple work-up procedure and the protocol provides a novel alternative for the synthesis of thioether.

[Design, synthesis and evaluation of new acetylcholinesterase inhibitors].

A series of novel 2-amino-4-phenylthiazole derivatives were designed and synthesized, furthermore, their inhibition effect on acetylcholinesterase were investigated. 2-Amino-4-phenylthiazoles were prepared from alpha-bromoacetophenones by Hantzsch reaction, acylation reaction and substitution reaction. Moreover, their bioactivities as AChE inhibitors in vitro were measured with Ellman spectrophotometry.

Synergism and rules of the new combination drug Yiqijiedu formulae (YQJD) on ischemic stroke based on amino acids (AAs) metabolism.

The use of combination drugs is considered to be a promising strategy to control complex diseases such as ischemic stroke. The detection of metabolites has been used as a versatile tool to reveal the potential mechanism of diverse diseases. In this study, the levels of 12 endogenous AAs were simultaneously determined quantitatively in the MCAO rat brain using RRLC-QQQ method.

DNA binding property and antitumor evaluation of xanthone with dimethylamine side chain.

In this work, a xanthone derivative was obtained by cationic modification of the free hydroxyl group of xanthone with dimethylamine group of high pKa value. The interactions of xanthones with DNA were investigated by spectroscopic methods, electrophoretic migration assay and polymerase chain reaction test. Results indicate that xanthones can intercalate into the DNA base pairs by the hydrophobic plane and the xanthone with dimethylamine side chain may also bind the DNA phosphate framework by the basic amine alkyl chain, thus showing a better DNA binding ability than the xanthone.

Dispersive solid-phase extraction based on magnetic dummy molecularly imprinted microspheres for selective screening of phthalates in plastic bottled beverages.

A new magnetic dummy molecularly imprinted dispersive solid-phase extraction (MAG-MIM-dSPE) coupled with gas chromatography-FID was developed for selective determination of phthalates in plastic bottled beverages. The new magnetic dummy molecularly imprinted microspheres (MAG-MIM) using diisononyl phthalate as a template mimic were synthesized by coprecipitation coupled with aqueous suspension polymerization and were successfully applied as the adsorbents for MAG-MIM-dSPE to extract and isolate five phthalates from plastic bottled beverages. Validation experiments showed that the MAG-MIM-dSPE method had good linearity at 0.

Preparation and characterization of poly(triallyl isocyanurate-co-trimethylolpropane triacrylate) monolith and its applications in the separation of small molecules by liquid chromatography.

A new polymeric monolith was prepared in stainless-steel column and fused-silica capillary, respectively, by atom transfer radical polymerization technique. In the polymerization, triallyl isocyanurate (TAIC) was used as the functional monomer; trimethylolpropane triacrylate (TMPTA) as the crosslinking agent; polyethylene glycol 200 and 1,2-propanediol as the co-porogens; carbon tetrachloride as the initiator and ferrous chloride as the catalyst. The conditions of polymerization were optimized.

Preparation of a novel porous poly (trimethylol propane triacrylate-co-ethylene dimethacrylate) monolithic column for highly efficient HPLC separations of small molecules.

A novel poly (trimethylol propane triacrylate-co-ethylene dimethacrylate) [poly (TMPTA-co-EDMA)] monolith was prepared by in situ free-radical polymerization in a 50 mm × 4.6mm i.d.

Preparation of a tetrazolyl monolithic column via the combination of ATRP and click chemistry for the separation of proteins.

Tetrazolyl monolithic column is first prepared through the combination of atom transfer radical polymerization (ATRP) and "click chemistry" technique. In the ATRP fabrication process, vinyl ester resin is used as both the monomer and the cross-linking agent, and cetyl alcohol is used as the porogen, carbon tetrachloride as the initiator and ferrous chloride as the catalyst. The monolith is modified by click chemistry, which forms the tetrazolyl monolithic column.

High-performance liquid chromatography separation of small molecules on a porous poly (trimethylol propane triacrylate-co-N-isopropylacrylamide-co-ethylene dimethacrylate) monolithic column.

A porous monolith was prepared by in situ free-radical polymerization using N-isopropylacrylamide (NIPAAm) and trimethylol propane triacrylate (TMPTA) as functional monomers, ethylene dimethacrylate (EDMA) as crosslinking agent. The chemical group of the monolith was assayed by a Fourier transform infrared spectroscopy (FT-IR) method and the morphology of optimized monolithic column was characterized by scanning electron microscopy (SEM). The mechanical strength and permeability have been studied in detail as well.

Synthesis and pharmacological evaluation of novel bisindolylalkanes analogues.

In an effort to develop potent anti-cancer chemopreventive agents that act on topoisomerase II, a novel series of bisindolylalkanes analogues such as 3,3'-(thiochroman-4,4-diyl)bis(1H-indole) are synthesized. Structures of all compounds are elucidated by (1)H NMR, (13)C NMR and HRMS. Anti-proliferative activities for all of these compounds are investigated by the method of MTT assay on 7 human cancer lines.

[Applications of polymeric monoliths in separation of bio-macromolecules].

In recent years, the applications of high performance liquid chromatographic polymeric monoliths in the separation of macromolecules have been developed. In the review, the characters and new developments of bio-macromolecules separation by using the polymeric monoliths, combining with the works in our laboratory are summarized. Moreover, related influential reports are referred.

Analysis of serum metabolites for the discovery of amino acid biomarkers and the effect of galangin on cerebral ischemia.

Ischemic stroke, a devastating disease with a complex pathophysiology, is a leading cause of death and disability worldwide. In our previous study, we reported that galangin provided direct protection against ischemic injury and acted as a potential neuroprotective agent. However, its associated neuroprotective mechanism has not yet been clarified.

The fabrication of monolithic capillary column based on poly (bisphenol A epoxy vinyl ester resin-co-ethylene glycol dimethacrylate) and its applications for the separation of small molecules in high performance liquid chromatography.

A new polymeric monolith was synthesized in fused-silica capillary by in situ polymerization technique. In the polymerization, bisphenol A epoxy vinyl ester resin (VER) was used as the functional monomer, ethylene glycol dimethacrylate (EDMA) as the crosslinking monomer, 1,4-butanediol, 1-propanol and water as the co-porogens, and azobisisobutyronitrile (AIBN) as the initiator. The conditions of polymerization have been optimized.

[Determination of endogenous amino acids in brain tissues after cerebral ischemia by RRLC-QQQ].

Objective: To establish a method to determine underivatized endogenous amino acids in brain tissues after cerebral ischemia based on RRLC-QQQ.

Method: Diamonsil chromatographic column C18 (4.6 mm x 250 mm, 5 microm) was adopted to determine 12 amino acids in 15 min, with acetonitrile-0.

On-line solid phase extraction using organic-inorganic hybrid monolithic columns for the determination of trace β-lactam antibiotics in milk and water samples.

A rapid and simple method with on-line solid phase extraction (SPE) has been developed for the simultaneous determination of beta-lactam antibiotics (BLAs) (amoxicillin, cephradine, and cefazolin sodium) in aquatic environment and milk. The epoxy-based organic-inorganic hybrid monolithic column was used as SPE sorbent to simultaneously monitor three analytes. The morphology of monolithic column and pressure drop across the columns were characterized.

An ion-pair principle for enantioseparations of basic analytes by nonaqueous capillary electrophoresis using the di-n-butyl L-tartrate-boric acid complex as chiral selector.

A chiral recognition mechanism of ion-pair principle has been proposed in this study. It rationalized the enantioseparations of some basic analytes using the complex of di-n-butyl l-tartrate and boric acid as the chiral selector in methanolic background electrolytes (BGEs) by nonaqueous capillary electrophoresis (NACE). An approach of mass spectrometer (MS) directly confirmed that triethylamine promoted the formation of negatively charged di-n-butyl l-tartrate-boric acid complex chiral counter ion with a complex ratio of 2:1.

[Advance of studies on metabolic fingerprinting analytical techniques and data processing methods].

Metabolomics is an emerging discipline subsequent to genomics, transcriptomics and proteomics, aiming for systematically studying the regularity of changes in metabolite to revealing organism's nature of movement and metabolism. It is especially important in modern pharmacological studies. Metabolic fingerprinting analysis is a method for metabolic analysis on high throughput of all metabolites, studying changes in drugs, organisms and endogenic metabolites caused by drugs and finding out related biomarkers to reflect dynamic changes inside organisms more directly and explain the mechanism of drugs and their effects on diseases.

Miniaturized molecularly imprinted matrix solid-phase dispersion coupled with high performance liquid chromatography for rapid determination of auxins in orange samples.

A simple, convenient and high selective miniaturized molecularly imprinted matrix solid-phase dispersion (mini-MI-MSPD) technique using l-tryptophan-imprinted polymers as sorbents was proposed for simultaneous extraction of four auxins (indole-3-acetic acid (IAA), indole-3-propionic acid (IPA), indole-3-butyric acid (IBA) and 1-naphthaleneacetic acid (NAA)) from orange samples coupled with high performance liquid chromatography-ultraviolet detection. The molecularly imprinted polymers (MIPs) synthesized using l-tryptophan as dummy template showed high affinity and selectivity to auxins, and so they were applied as the specific dispersant of MSPD to simultaneously eliminate the effect of template leakage on quantitative analysis. Under the optimized conditions, good linearity was obtained in a range of 0.

Ultrasound-assisted extraction of syringin from the bark of Ilex rotunda thumb using response surface methodology.

In this work, a rapid extraction method based on ultrasound-assisted extraction (UAE) of syringin from the bark of Ilex rotunda Thumb using response surface methodology (RSM) is described. The syringin was analyzed and quantified by high performance liquid chromatography coupled with UV detection (HPLC-UV). The extraction solvent, extraction temperature and extraction time, the three main factors for UAE, were optimized with Box-Behnken design (BBD) to obtain the highest extraction efficiency.

[Design, synthesis and in vitro antifungal activity of 3-substituted-methylenechroman-4-ones].

Substituted phenols as the starting materials were transformed into substituted chromanones by substitution reaction and cyclization reaction, and then 3-(hydroxymethylene)chroman-4-ones were synthesized from substituted chromanones by condensation reaction; at last, the target compounds were synthesized from 3-(hydroxymethylene)chroman-4-ones by chlorination reaction. Their structures were confirmed by 1H NMR and MS. The antifungal activity of the target compounds in vitro was measured by consecutive double dilution, and the result of antifungal experiment indicated that the target compounds had good antifungal action on most fungi tested in vitro.

[Chiral separation of five beta-blockers using di-n-hexyl L-tartrate-boric acid complex as mobile phase additive by reversed-phase liquid chromatography].

A reversed-phase high performance liquid chromatographic (HPLC) method using the di-n-hexyl L-tartrate-boric acid complex as a chiral mobile phase additive was developed for the enantioseparation of five beta-blockers including propranolol, esmolol, metoprolol, bisoprolol and sotalol. In order to obtain a better enantioseparation, the influences of concentrations of di-n-butyl L-tartrate and boric acid, the type, concentration and pH of the buffer, methanol content as well as the molecular structure of analytes were extensively investigated. The separation of the analytes was performed on a Venusil MP-C18 column (250 mm x 4.

In situ synthesis of twelve dialkyltartrate-boric acid complexes and two polyols-boric acid complexes and their applications as chiral ion-pair selectors in nonaqueous capillary electrophoresis.

In this paper, twelve dialkyltartrate-boric acid complexes and two polyols-boric acid complexes were in situ synthesized by the reaction of different dialkyltartrates or polyols with boric acid in methanol containing triethylamine. All of the twelve dialkyltartrate-boric acid complexes were found to have relatively good chiral separation performance in nonaqueous capillary electrophoresis (NACE). Their chiral recognition effects in terms of both enantioselectivity (α) and resolution (R(s)) were similar when the number of carbon atoms was below six in the alkyl group of alcohol moiety.