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- Author or Editor: W. Liu x
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Summary
10-O-(N,N-dimethylaminoethyl)-ginkgolide B (XQ-1) is an intermediate for synthesizing 10-O-(N,N-dimethylaminoethyl)-ginkgolide B methanesulfonate (XQ-1H), which is a novel ginkgolide B derivative and is being developed as a platelet-activating factor antagonist. A specific and rapid liquid chromatographic method was developed for the quantitative analysis of XQ-1 and its three related impurities, which were 10-O-(N,N-dimethylaminoethyl)-11,12-seco-ginkgolide B (imp-1), 10-O-(N,N-dimethylaminoethyl)-11,12-seco-3,14-dehydroginkgolide B (imp-2) and 10-O-(N,N-dimethylaminoethyl)-3,14-dehydroginkgolide B (imp-3) simultaneously in XQ-1 samples. Chromatographic separation was achieved on a CN band stationary phase, with the mobile phase consisting of methanol and 20 mM dipotassium hydrogen phosphate (pH 7.5) (50:50, υ/υ) in isocratic elution. The flow rate was 1.0 mL min−1 and detector was set at 220 nm. The method was optimized by the analysis of the samples generated during the forced degradation studies. The XQ-1, imp-1, imp-2, and imp-3 were completely separated within 15 min. The resolutions (R s) amongst four target compounds were >2. The developed method was validated with respect to specificity, linearity, accuracy, precision, and robustness. The results indicated that the simultaneous LC determination method was readily utilized as a quality control method for XQ-1 sample.
Summary
A preparative high-speed countercurrent chromatograph (HSCCC) method for the isolation and purification of C6-C2 natural alcohol and benzyl ethanol from Forsythia suspensa was successfully established. Cornoside, forsythenside F, forsythiaside, and acteoside were rapidly obtained for the first time by HSCCC with a two-phase solvent system ethyl acetate-n-butanol-methanol-water (5:1:0.5:5, υ/υ) in one-step separation. The purities of them were all above 97% as determined by high-performance liquid chromatography, and the combination of ESI-MS and NMR analysis confirmed the chemical structures of the four compounds.
Summary
A simple and rapid HPLC method using a photodiode array (PDA) detector for the analysis of 3-hydroxycarboplatin and its related complex has been established for the first time. Separation of 3-hydroxycarboplatin and 3-hydroxy-1,1-cyclobutanedicarboxylic acid (3-HO-cbdca) was carried out on a Phenomenex ODS3 column using an aqueous solution containing 50 mM ammonium acetate and 5 mM sodium 1-octanesulfonate as the mobile phase. The flow rate was 0.8 mL min−1, the column temperature was 40°C, and the detection wavelength was 230 nm for 3-hydroxycarboplatin and 220 nm for 3-HO-cbdca. Different analytical performance parameters such as precision, accuracy, linearity, stability of the solution, specificity, limit of detection (LOD), limit of quantification (LOQ), and system suitability were determined using the Empower 2 software. The calibration curve of standard 3-hydroxycarboplatin showed good linearity (r = 0.9995) within the range 0.5–1.4 mg mL−1. The method was accurate and precise, with an average accuracy of 100.4% (RSD = 1.53%, n = 9), and the results of the system suitability test showed symmetrical peaks, good resolution (R s), and repeatability. It can be applied to the quality control of 3-hydroxycarboplatin.
Abstract
Thermogravimetry (TG) was employed to study the thermal degradation kinetics of poly(etherketone/sulfone)ethylimide (PEK-IE and PES-IE). The corresponding decomposition activation energies and reaction orders were obtained and the comparison was made with their parent polymerspoly(ether-ketone/sulfone) with Cardo group (PEK-C and PES-C). The results show that the degradation activation energies of PEK-IE and PES-IE were lower than that of PEK-C and PES-C; and two stages of the degradation process were found for all the four polymers. For PEK-IE and PES-IE, the activation energies in the first decomposition stage are much lower than that in the second stage and the two stages can be taken as slow induction and fast degradation, whereas for PEK-C and PES-C the activation energies in the first decomposition stage are larger than that in the second stage, and the two stages can both be taken as two fast degradation stages. The decomposition mechanism of the two stages was also speculated.
Summary Samples of electrolytic manganese dioxide (EMD) were chemically reduced using 2-propanol under reflux (82°C) for 1, 2, 3, 6 and 24 h intervals. XRD analysis showed that the ?-MnO2 structure was preserved although the lattice dimensions were observed to increase with increasing degree of reduction to accommodate the intercalation of protons. The exception was the 24 h reduced sample which contained two phases; ? -MnO2 and ? -MnOOH. Three regions of decomposition in the range of 50 to 1000°C were observed using thermogravimetric analysis coupled with mass spectrometry (TG-MS) and were accounted for as water removal below 390°C, reduction of MnO2 to Mn2O3 between 400 and 600°C, and Mn2O3 to Mn3O4 between 600 and 1000°C. Again the exception proved to be the 24 h reduced sample which was observed to decompose predominantly in one step between 400 and 600°C directly to Mn3O4.
Abstract
Pb(1,4-BDC)·(DMF)(H2O) (1,4-BDC=1,4-benzenedicarboxylate; DMF=dimethylformamide) has been synthesized and investigated by elemental analysis, FTIR spectroscopy, thermogravimetry (TG), derivative thermogravimetry (DTG). TG-DTG curves show that the thermal decomposition occurs in four stages and the corresponding apparent activation energies were calculated with the Ozawa-Flynn-Wall (OFW) and the Friedman methods. The most probable kinetic model function of the dehydration reaction of the compound has been estimated by the Coats-Redfern integral and the Achar-Bridly-Sharp differential methods in this study.
Red coleoptile is an easily observed agronomic trait of wheat and has been extensively studied. However, the molecular mechanism of this trait has not yet been revealed. In this study, the MYB gene TaMYB-D1 was isolated from the wheat cultivar ‘Gy115’, which possesses red coleoptiles. This gene resided at the short arm of the homoelogous group 7 chromosomes. TaMYB-D1 was the only gene expressed in the coleoptiles of ‘Gy115’ and was not expressed in ‘Opata’ and ‘CS’, which have uncoloured coleoptiles. Phylogenetic analysis placed TaMYB-D1 very close to ZmC1 and other MYB proteins regulating anthocyanin biosynthesis. The encoded protein of TaMYB-D1 had an integrated DNA binding domain of 102 amino acids and a transcription domain with 42 amino acids, similar to the structure of ZmC1. Transient expression analysis in onion epidermal cells showed that TaMYB-D1 was located at the plant nucleus, which suggested its role as a transcription factor. The expression of TaMYB-D1 was accompanied with the expression of TaDFR and anthocyanin biosynthesis in the development of the coleoptile of ‘Gy115’. Transient expression analysis showed that only TaMYB-D1 induced a few ‘Opata’ coleoptile cells to synthesize anthocyanin in light, and the gene also induced a colour change to red in many cells with the help of ZmR. All of these results suggested TaMYB-D1 as the candidate gene for the red coleoptile trait of ‘Gy115’.
Barley stripe mosaic virus (BSMV)-based virus induced gene silencing (VIGS) is an effective strategy for rapid determination of functional genes in wheat plants. ERECTA genes are reported to regulate stomatal pattern of plants, and manipulation of TaERECTA (a homologue of ERECTA in bread wheat) is a potential route for investigating stomatal development. Here, the leucine-rich repeat domains (LRRs) and transmembrane domains of TaERECTA were selected to gain BSMV:ER-LR and BSMV:ER-TM constructs, respectively, targeting TaERECTA for silencing in wheat cultivars ‘Bobwhite’ and ‘Cadenza’, to identify the function of TaERECTA on stomatal patterns. The results showed that reduced expression of TaERECTA caused an increased stomatal and epidermal cell density by average 13.5% and 3.3%, respectively, due to the significantly reduced size of leaf epidermal and stomatal cells, and this led to an increase in stomatal conductance. These suggest that modulation of TaERECTA offers further opportunities in stomatal engineering for the adaptation of photosynthesis in wheat.
Gibberellins (GAs) are a class of plant hormones that play important roles in diverse aspects during plant growth and development. A series of GA synthesis and metabolism genes have been reported or proved to have essential functions in different plant species, while a small number of GA 2-oxidase genes have been cloned or reported in wheat. Previous studies have provided some important findings on the process of GA biosynthesis and the enzymes involved in its related pathways. These may facilitate understanding of the complicated process underlying GA synthesis and metabolism in wheat. In this study, GA 2-oxidase genes TaGA2ox1-1, TaGA2ox1-2, TaGA2ox1-3, TaGA2ox1-4, TaGA2ox1-5, and TaGA2ox1-6 were identified and further overexpressed in rice plants to investigate their functions in GA biosynthesis and signaling pathway. Results showed overexpression of GA 2-oxidase genes in rice disrupted the GA metabolic pathways and induced catalytic responses and regulated other GA biosynthesis and signaling pathway genes, which further leading to GA signaling disorders and diversity in phenotypic changes in rice plants.
Leaf senescence is a notably important trait that limits the yield and biomass accumulation of agronomic crops. Therefore, determining the chromosomal position of the expression sequence tags (ESTs) that are associated with leaf senescence is notably interesting in the manipulation of leaf senescence for crop improvement. A total of 32 ESTs that were previously identified during the delaying leaf senescence stage in the stay-green wheat cultivar CN17 were mapped to 42 chromosomes, a chloroplast, a mitochondrion, and a ribosome using in silico mapping. Then, we developed 19 pairs of primers based on these sequences and used them to determine the polymorphisms between the stay-green cultivars (CN12, CN17, and CN18) and the control cultivar MY11. Among the 19 pairs of primers, 5 pairs produced polymorphisms between the stay-green cultivar and the non-stay-green control. Further studies of Chinese Spring nullisomic-tetrasomics show that JK738991 is mapped to 3B, JK738983 is mapped to 5D, and JK738989 is mapped to 2A, 4A, and 3D. The other two ESTs, JK738994 and JK739003, were not assigned to a chromosome using the Chinese Spring nullisomic-tetrasomics, which indicates that these ESTs may be derived from rye DNA in the wide cross. In particular, the ESTs that produce polymorphisms are notably useful in identifying the stay-green cultivar using molecular marker-assisted selection. The results also suggest that the in silico mapping data, even from a comparison genomic analysis based on the homogeneous comparison, are useful at some points, but the data were not always reliable, which requires further investigation using experimental methods.
