Two complexes based on the ligand 1,4‐dihydro‐2,3‐quinoxalinedione, namely [Mn(H2L)2(H2O)2]n ( 1 ) and {[Zn2(H2L)2(tz)2] · 5H2O}n ( 2 ) (H3L = 2,3‐dioxo‐1,2,3,4‐tetrahydroquinoxaline‐6‐carboxylic acid, Htz = 1,2,4‐triazole) were hydrothermally synthesized and characterized by elemental analyses, IR spectroscopy, as well as single‐crystal and powder X‐ray diffraction. Complex 1 exhibited a 1D comb‐like chain formed by H2L– anions linking MnII ions, whereas complex 2 was a 2D layer‐like structure with square‐shaped windows and outstretched arms built by combination of H2L– and tz– ligands with ZnII ions. The adjacent chains or layers connected with each other by intermolecular hydrogen bonding and π–π stacking to further extend to a 3D supermolecular framework. In addition, the thermal stabilities, luminescence properties, and optical energy gap of 1 and 2 were investigated in detail. 相似文献
An off-line orthogonal two-dimensional preparative liquid chromatography method was developed for isolation of high-purity compounds from aqueous extracts of Pinus massoniana Lamb., which has efficient therapeutic properties in recipes of traditional Chinese medicines. A polar-enhanced reversed-phase (RP) column, XAqua C18 was selected for the first-dimensional separation. A HILIC column and a hydrophobic RP column were both explored in the second dimension. The preparation results indicated hydrophilic RP × HILIC mode would provide better separation efficiency for polar complexes, i.e., the second-dimensional separation was finished in less than 30 min and high-purity compounds were obtained. In this work, 16 fractions were collected efficiently in the first dimension with a recovery up to 96%, and six compounds with high purity and enough quantity were identified by NMR and high resolution mass spectrometry, including epicatechin, betuloside, taxifolin-3-O-xyloside, cedrusin-4-O-glucoside, massonianoside C and massonianoside D, and five are glycosides, including flavonoid glycosides, lignanoid glycosides and an arylbutanoid glycoside. Betuloside was first reported in the preparation of Pinus massoniana Lamb. This work demonstrated a flexible strategy of compromise in between time and resolution for selecting solvent and column to enhance preparative efficiency of polar complex systems. 相似文献
The authors describe a signal amplification strategy for highly sensitive detection of the prostate-specific antigen (PSA). This is accomplished by a combination of two methods, viz. (a) improved surface-initiated enzymatic polymerization (SIEP), and (b) the use of nanoflowers prepared from C60 fullerene and Methylene Blue (C60/MB) modified with a long single-strand DNA. C60/MB acts as a novel electrochemical indicator. The C60/MB nanoflowers improve the load of MB and promote the electron transfer. The integration of the SIEP technique and the C60/MB nanomaterial also results in improved loading of MB on the nucleic acid. Ultimately, dual cascade signal amplification is accomplished. The biosensor was constructed as follows: (a) Gold nanospheres were modified with antibody 2 (Ab2) and a thiolated oligonucleotide (referred to as S0). (2) S0 is then extended by the SIEP reaction. (3) The redox indicator C60/MB is then connected to the extended guanine-rich ssDNA which then yields the amperometric signal. (4) A sandwich immunoassay is performed by capturing the nanoprobe oy type Ab2-Au-S0 on the gold electrode modified with multi-walled carbon nanotubes (MWCNTs) and protein A. Current is measured by using differential pulse voltammetry (DPV). The synergic effect of the biofunctional nanomaterial and the signal amplification strategy greatly improves the performance of this immunoassay. Under optimized conditions and at a working voltage of typically ?0.18 V (vs Ag/AgCl), the assay has a linear range that extends from 15 pg·mL?1 to 8 ng·mL?1 of PSA. The detection limit is as low as 1.7 pg·mL?1 (at an S/N ratio of 3). In our perception, this dual amplification scheme has a wide scope in that it may become applicable to numerous other immunoassays.
Graphical abstract C60/Methylene blue nanoflowers, a novel electrochemical indicator, connect with the long single-stranded DNA (ssDNA) extended by the improved surface-initiated enzymatic polymerization method. This amplification strategy is utilized to construct a sandwich prostate-specific antigen (PSA) immunosensor.
30R- and 30S-oxazoline analogues of apratoxin E have been prepared with late-stage formation of an oxazoline ring. These two compounds have a potent inhibitory effect on HCT-116 cell proliferation with IC50 values of 345 and 638 nM, respectively. These results suggest that apratoxin E oxazoline bioisosteres are approximately 6-fold less potent than their thiazoline parent compounds. A positive impact of the 30R conformation on antiproliferative activity was also observed, with approximately 2-fold enhancement when compared to the 30S epimer. 相似文献