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981.
Xiuhui He Zhaohong Su Qingji Xie Chao Chen Yingchun Fu Li Chen Ying Liu Ming Ma Le Deng Dilan Qin Yueping Luo Shouzhuo Yao 《Mikrochimica acta》2011,172(1-2):95-102
A simple, cheap, and nonpolluting method was developed for the cloud point extraction of gold (Au) and palladium (Pd). It is based on the complexation reaction of Au and Pd with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) and micelle mediated extraction of the complex using the non-ionic surfactant poly(ethylene glycol) mono-p-nonylphenyl ether (PONPE 7.5). Under the optimized experimental conditions, the enrichment factors are 16 and 17 for Au and Pd, respectively, for 15?mL of preconcentrated solution. The limits of detection are 3.8???g?L?1 and 1.8???g?L?1 for Au and Pd, respectively. The relative standard deviations are 1.4% for Au and 0.6% for Pd (n?=?11). The method was successfully applied to the determination of Au and Pd in certified reference materials and mine samples. Figure
CPE of gold(III) and palladium(II) 相似文献
982.
A simple hydrophilic-interaction chromatography (HILIC) method was developed for the identification and quantification of 14 nucleosides and nucleobases, namely cytosine, uracil, cytidine, guanine, hypoxanthine, xanthine, uridine, thymine, inosine, guanosine, thymidine, 2′-deoxyadenosine, 2′-deoxyinosine and 2′-deoxyuridine in two traditional Chinese medicines, Geosaurus and Leech. The separation was achieved on a TSKgel Amide-80 column (150 mm × 2.0 mm, 3.0 μm) with a mixture of acetonitrile and 10 mM aqueous ammonium acetate as the mobile phase at a flow rate of 0.2 mL/min. The temperature was set at 30 °C and UV detection wavelength was set at 260 nm. All calibration curves showed good linearity (R2 > 0.9957) within the test ranges. The overall intra- and inter-day RSD ranged from 0.4 to 3.4% and from 0.7 to 3.3%, respectively. The LOD and LOQ were in the range of 0.07-30.49 ng/mL and 0.26-60.98 ng/mL, respectively. The repeatability of the method was in the range of 2.2-5.8% for Geosaurus and 1.4-5.5% for Leech. The recoveries of the samples were in the range of 91.4-100.9% for Geosaurus, and 91.9-99.3% for Leech. The established method was applied successfully for the analysis of nucleosides and nucleobases in 22 commercially available samples collected from different regions in China and Japan. Our data showed that HILIC had advantages as a useful tool for the study of the bioactive components in Geosaurus and Leech as well as their quality control, and could therefore be used for the determination of the analytes in pharmaceutical products and biological fluids. 相似文献
983.
The N-terminal valine adduct (HETE-Val) in globin is believed to behave as a long-lived biomarker after exposure to sulfur mustard (HD). Development of a highly sensitive method for monitoring HETE-Val, particularly at low HD exposure levels or for retrospective detection, would be a significant achievement. In this study, by improving the sample preparation method, a sensitive NCI-GC/MS method was established for the analysis of HETE-Val in globin after HD exposure. To optimize and investigate the sample preparation method, all the relevant HETE-Val chemicals were synthesized, purified, and characterized. By carrying out optimized solid phase extraction (SPE) cleanup followed by modified Edman degradation results in a low detection level and clean baseline. The minimum detectable exposure level of human blood (in vitro) to HD is 20 nmol/L (S/N > 3). The interday and intraday precisions of the proposed method were found to be acceptable with less than a 15% relative standard deviation (RSD). A nearly linear dose-effect relationship was observed between HETE-Val and a HD exposure concentration range of 0.1-120 μmol/L. The percentage of HD that reacted with N-terminal valine in globin obtained from human blood (in vitro) was quantified using the proposed method. 相似文献
984.
Thin wall samples of high density polyethylene (HDPE) were prepared via injection molding with different injection speeds ranging from 100 mm/s to 1200 mm/s. A significant decrease in the tensile strength and Young??s modulus was observed with increasing injection speed. In order to investigate the mechanism behind this decrease, the orientation, molecular weight, molecular weight distribution, melt flow rate, crystallinity and crystal morphology of HDPE were characterized using two-dimensional wide-angle X-ray diffraction (2D-WAXD), gel permeation chromatography (GPC), capillary rheometry and differential scanning calorimetry (DSC), respectively. It is demonstrated that the orientation, molecular weight, molecular weight distribution, melt flow rate and crystallinity have no obvious change with increasing injection speed. Nevertheless, the content of extended chain crystals or large folded chain crystals was found to decrease with increasing injection speed. Therefore, it is concluded that the decrease in tensile properties is mainly contributed by the reduced content of extended chain crystals or large folded chain crystals. This study provides industry with valuable information for the application of high speed injection molding. 相似文献
985.
Zhang ST Fang HM Zhao L Tian QN Qin YF Lu P Chen SJ Bao ZX Liang F 《Applied biochemistry and biotechnology》2011,164(7):1037-1047
Ancrod, a serine protease purified from the venom of Agkistrodon rhodostoma, is highly specific for fibrinogen. It causes anticoagulation by defibrinogenation and has been used as a therapeutic anticoagulant for the treatment of moderate to severe forms of peripheral arterial circulatory disorders in a variety of countries. The DNA of ancrod was amplified by recursive PCR with a yeast bias codon and cloned into the pGEM-T Easy vector. In order to achieve a high level secretion and a full activity expression of ancrod in Pichia pastoris (P. pastoris), the P. pastoris protein disulfide bond isomerase (PpPDI) was co-overexpressed in the strain. The secretion characteristics of ancrod with and without PpPDI were examined. With co-overexpression of PpPDI, the production of recombinant ancrod (rAncrod) was increased to 315 mg/L in the culture medium, which is twofold higher than the control strain carrying only the ancrod gene. Through purified by Ni2? affinity chromatography and phenyl Sepharose column, the purity of rAncrod was found to be as high as 95.2%. The fibrinogenolytic and zymographic activities of the rAncrod were determined and found to be similar to that of the native protein. This improved expression system can facilitate further studies and the industrial production of ancrod. 相似文献
986.
Qin Y Zhang Y He H Zhu J Chen G Li W Liang Z 《Applied biochemistry and biotechnology》2011,163(8):1012-1019
After screening with 0.1% esculoside and 0.03% FeCl3, we identified from rotten wood a fungal isolate HML0366 that produces high amount of β-glucosidase. Phenotypic and rDNA
internal transcribed spacer sequence analyses indicated that the isolate belongs to Aspergillus oryzae. The β-glucosidase produced by HML0366 had an activity of 128 U/g. high performance liquid chromatography analysis also demonstrated
a high transglycosylation activity of the crude enzyme. The β-glucosidase was stable between pH 4–10 at 60 °C. A gentiobiose
yield of 30.86 g/L was achieved within 72 h of the enzymatic reaction at pH 5 and 55 °C using 50% glucose as the substrate.
For the first time, we report here the isolation of an A. oryzae strain producing β-glucosidase with high hydrolytic activities. The crude enzyme has a high transglycosylation activity,
which enables the enzymatic synthesis of gentiooligosaccharides. 相似文献
987.
Dried blood spot (DBS) technology is an emerging alternative for sample collection in bioanalysis. Dilution for DBS samples is a challenge due to its solid sample format. Currently, DBS samples requiring dilution were first extracted as regular samples and then diluted with extracted blank samples containing internal standard (IS). Since the dilution step is a volume-critical step, extra care has to be taken to achieve accurate dilution when dealing with limited volume extracted samples. Here, we introduce an alternative sample dilution for liquid chromatography/tandem mass spectrometry (LC/MS/MS) assays using IS to track the dilution step. Dilution factor-adjusted IS working solution was first added to the sample requiring dilution before sample processing; subsequently, the processed sample was approximately diluted into the assay linear response range before LC/MS/MS analysis. We define this approach as "IS-tracked dilution". The advantage of this approach is that the diluting step is tracked by the IS and is no longer a volume-critical step. Another recognized challenge related to sample dilution is automatic sample dilution using a liquid handler. This "IS-tracked dilution" may also help address some of the challenges for automatic sample dilution of liquid samples. This new dilution approach was proven to be effective and convenient in both plasma assays and DBS assays using omeprazole as a probe compound. 相似文献
988.
989.
Lei Liu Jing Li Mingan Wang Fengpei Du Zhaohai Qin Bin Fu 《Tetrahedron: Asymmetry》2011,22(5):335-557
A series of novel heteroarylidene malonate derived bis(thiazoline) ligands 1 and 2 were synthesized and applied to a Friedel-Crafts reaction between indole and alkylidene malonate. The Cu(OTf)2 complex of ligand 2b bearing a benzyl group afforded moderate to excellent enantioselectivity for the adducts (up to >99% ee). 相似文献
990.
Cellulose films were successfully prepared from NaOH/urea/zincate aqueous solution pre-cooled to −13 °C by coagulating with
5% H2SO4. The cellulose solution and regenerated cellulose films were characterized with dynamic rheology, ultraviolet–visible spectroscope,
scanning electron microscopy, wide angle X-ray diffraction, Fourier transform infrared (FT-IR) spectrometer, thermogravimetry
and tensile testing. The results indicated that at higher temperature (above 65 °C) or lower temperature (below −10 °C) or
for longer storage time, gels could form in the cellulose dope. However, the cellulose solution remained a liquid state for
a long time at 0–10 °C. Moreover, there was an irreversible gelation in the cellulose solution system. The films with cellulose
II exhibited better optical transmittance, high thermal stability and tensile strength than that prepared by NaOH/urea aqueous
solution without zincate. Therefore, the addition of zincate in the NaOH/urea aqueous system could enhance the cellulose solubility
and improve the structure and properties of the regenerated cellulose films. 相似文献