Quantitative determination of soybean meal content in compound feeds: comparison of near-infrared spectroscopy and real-time PCR

Standard methods for determining the raw material content of compound feed are little exploited, except for the identification of meat and bone meal in feeds. In this work, near-infrared (NIR) spectroscopy and real-time polymerase chain reaction (PCR) were applied in order to establish new and fast methods for quantification of soybean meal content in compound feeds. The best prediction quality was achieved by using a model based on NIR spectroscopy (R ² = 0.9857, standard error of cross-validation 1.1065). Furthermore, a sensitive qualitative detection method by using the real-time PCR was developed (R ² = 0.976, slope −3.7599). Finally, the differences between the real-time PCR result and the NIR spectroscopy result for a given sample were also treated, and we found that the NIR spectroscopy method provided quite accurate results which approach closely those of the real-time PCR method. Hui Li and Xiaowen Lv contributed equally to this work.     

Simple, Sensitive and Rapid LC–ESI–MS Method for the Quantitation of Olprinone in Rat Plasma

Olprinone is a phosphodiesterase (PDE)-3 inhibitor. This paper describes a simple, selective and sensitive method for the quantification of olprinone in rat plasma using a liquid–liquid extraction procedure followed by liquid chromatography mass spectrometric (LC–MS) analysis. The method had an advantage of high sensitivity. Analyses were conducted at a flow rate of 0.25 mL min⁻¹ by a gradient elution. The detection utilized selected ion monitoring in the positive ion mode at m/z 251.0 and 344.0 for the protonated molecular ions of olprinone and the internal standard, respectively. The quantitation limit for olprinone in rat plasma was 0.5 ng mL⁻¹. The linearity was also excellent over the concentration range of 0.5–100 ng mL⁻¹ of olprinone. The intra- and inter-day precision (relative standard deviation (RSD) %) was lower than 10%, and accuracy ranged from 90 to 110%. This developed method was successfully applied to analysis of olprinone in biological fluids.     

木槿叶中混合氨基酸的提取工艺研究

以浓盐酸和乙醇溶液为提取剂,分别通过加热回流和超声波组织破碎法提取了木槿叶中的混合氨基酸,确定了氨基酸提取的最佳工艺条件。结果表明,用盐酸回流提取,盐酸与木槿干粉的液料比为25∶1,盐酸浓度6 mol/L,100℃下回流提取5 h,提取3次,氨基酸的提取效果最佳,提取率可达16.76%,产品收率可达8.6%。用80%乙醇溶液,室温下超声波提取30 min,提取3次,提取效果最好,提取率可达17.42%,产品收率可达8.93%。     

Effect of operating conditions on the removal of Pb2+ by microporous titanosilicate ETS-10 in a fixed-bed column

The breakthrough behavior of Pb2+ in an ETS-10 fixed bed was experimentally examined at various operating conditions. Results showed that the adsorption amount of Pb2+ ions per unit mass of ETS-10 particles in a column is about 1.68 mmol/g under the experimental conditions. This amount was not markedly affected by the operating conditions because of the rapid adsorption rate of Pb2+ ions on ETS-10. In the presence of competitive metal ions, the amount of Pb2+ adsorbed on ETS-10 was slightly reduced. An overshoot of the effluent concentrations of competitive metal ions Cu2+ and Cd2+ was observed in the adsorption systems of binary and ternary solutions. This is ascribed to the replacement of pre-adsorbed Cu2+ and Cd2+ ions by Pb2+ ions. The ETS-10 column broken up by Pb2+ ions can be regenerated by using an EDTA-Na2 solution and the regenerated column can be reused.     

At-line coupling of UPLC to chip-electrospray-FTICR-MS

Since highly sensitive on-line coupling of UPLC with FTICR-MS is technically infeasible due to their different scan rates, at-line coupling of these techniques was developed for rapid analysis. To enable cutting of one peak of the chromatogram into one fraction, several conditions and relationships were investigated, e.g. the optimum volume of the inserted delay loop, the relationship between retention time, loop outlet drop speed, individual drop volume versus mobile phase composition under constant speed, and linear solvent strength gradient elution modes. Good and reproducible results were achieved applying UPLC as an efficient separation and fast fractionation tool before the FTICR-MS measurements. A chip-based nanoelectrospray ionization system was employed which was perfectly suited to handling the small-volume fractions and was thus chosen for the at-line coupling. The method was initially applied to spiked extracts of cell-free bacterial culture supernatants in which bacterial signalling compounds, namely N-acyl homoserine lactones (AHL), were detected. Good reproducibility and high recovery was observed. Afterwards, a culture supernatant of Erwinia sp. JX3.2, a putative AHL producer, was investigated and N-hexanoyl-homoserine lactone was determined as a possible signalling molecule. More reliable assignments were achieved by use of at-line coupling of UPLC and FTICR-MS compared with off-line measurements. Xiaojing Li and Agnes Fekete have contributed equally to this publication.     

Synthesis, antiviral and antifungal bioactivity of 2-cyano-acrylate derivatives containing phosphonyl moieties

Alkyl 2-cyano-3-methylthio-3-phosphonylacrylates were synthesized by the reaction of alkyl 2-cyano-3,3-dimethylthioacrylates with dialkyl phosphites. The structures of the new compounds were characterized by elemental analyses, IR, 1H-, 13C- and 31P-NMR spectral data. These compounds were tested in vitro against pathogenic fungi, namely, Fusarium graminearum, Cytospora mandshurica and Fusarium oxysporum. Amongst all compounds, 2d and 2t were found to be effective against the tested fungi at 50 microg/mL. A half-leaf method was used to determine the in vivo protective, inactivation and curative efficacies of the title products against tobacco mosaic virus (TMV). Title compounds 2a and 2b were found to possess good in vivo curative, protection and inactivation effects against TMV with inhibitory rates at 500 mg/L of 60.0, 89.4 and 56.5 and 64.2, 84.2 and 61.2 %, respectively. To the best of our knowledge, this is the first report on the antiviral and antifungal activity of alkyl 2-cyano-3-methylthio-3-phosphonylacrylates.     

Antifungal activity of some diaryl ethers

Several diaryl ethers were synthesized and tested in vitro against seven phytopathogenic fungi, namely Fusarium graminearum, Alternaria alternate, Helminthosporium sorokinianum, Pyricularia oryzae, Fusarium oxysporum f. sp. vasinfectum, Fusarium oxysporum f. sp. cucumarinum and Alternaria brassicae. Compared to a commercial agricultural fungicide, hymexazol, especially compounds a, b, e, g and k were found to be more effective at 50 mug/ml against F. graminearum, F. oxysporum f. sp. vasinfectum and F. oxysporum f. sp. cucumarinum. Meantime, some structure-activity relationships were also observed.     

Controlled aggregation of functionalized gold nanoparticles with a novel conjugated oligomer.

A new route is developed to control the self-assembly of gold nanoparticles (AuNPs) functionalized with a novel pyridyl-ended porphyrin-oligo(p-phenylene vinylene) conjugated oligomer (P-OPV-Py) into branched-rods, chain-networks, uniform fractal-like Au clusters, and larger nanoparticles. The techniques of optical spectroscopy, transmission electron microscopy (TEM) and dynamic light scattering (DLS) are used to characterize the self-assembly in various solvent systems (pure toluene, CHCl(3)/toluene, THF/toluene and n-butanol/toluene). A combination of the ligand/AuNPs molar ratio and relative concentration serves as the driving force to control the size and shape of P-OPV-Py capped AuNPs.     

伐地那非的合成工艺改进

以2-乙氧基苯腈为原料,依次经Pinner反应和肼解反应制得中间体2-乙氧基苯甲亚胺酸酰肼（3）; 3经两步环合,氯磺化和氨化反应制得伐地那非,其结构经¹H NMR, ¹³C NMR和MS（ESI）确证,总收率31.6%。     

Porous graphene oxide-based carbon artefact with high capacity for methylene blue adsorption

A three-dimensional porous graphene oxide (PGO) material prepared by hydrothermal method was selected to adsorb methylene blue (MB), which demonstrates a high MB adsorption capacity, up to 1100 mg g^?1 in alkaline solution at room temperature. The influences of different pore structures and different contents of oxygen-containing functional groups on MB adsorption behaviors were studied in detail, which indicated that the high MB adsorption capacity is mainly ascribed to the synergistic effect of the large number of oxygen-containing functional groups and the interconnected 3D porous network. Moreover, based on the investigation on the adsorption kinetics and the effect of pH value on MB adsorption, we propose a two-step adsorption kinetics for PGO, which involved in two interactions between MB molecular and porous graphene oxide-based carbon: electrostatic force and π-π stacking. Besides, the calculation of the activation energies indicates that chemisorption dominates the adsorption for PGO in comparison with physisorption for three-dimensional porous graphene materials which has low adsorption capacity because of the removal of functional groups. The results are of great significance for the design and environmental applications of PGO as a promising adsorbent material for water purification.