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Summary

Two rapid, sensitive and reproducible methods for the determination of baclofen(BAL) in urine and plasma based on high-performance liquid chromatography (HPLC) with UV-vis and fluorescent detection, respectively, were developed for the first time using a new synthesized fluorescent label, 6-oxy-(N-succinimidylacetate)-9-(2′-methoxycarbonyl) fluorescein (SAMF). The optimal derivatization yield was achieved in borate buffer (pH 8.0) for 15 min at room temperature (25 °C). With a mixture of methanol and water containing 5 mmol L−1 sodium citrate buffer (pH 5.0) as mobile phase, BAL was determined at λ = 455 nm with UV-vis detection and at λ ex/λ em = 488/520 nm with FD detection. The detection limits are 1.065 × 10−3 mg mL−1 and 1.065 × 10−2 mg mL−1 with HPLC-UV-vis and HPLC-FD, respectively. The proposed method has been successfully applied to the analysis of BAL in human urine and plasma samples. The established method is rapid (15 min of derivatization process and 10 min of chromatographic run), reproducible and sensitive.

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Summary

A reversed-phase high-performance liquid chromatographic method was developed for the first time to simultaneously determine salicin and eight flavonoids in leaves of Salix matsudana, that is salicin, luteolin-7-O-glucoside, myricetin, apigenin-3′-oxyethyl-7-O-glucoside, rutin, quercetin, luteolin, kaempferol and apigenin. The separation of these compounds was achieved on a reversed phase C18 column (250 × 4.6 mm, 5 μm), with linear gradient of methanol in 0.2% phosphoric acid solution with a flow rate of 1.0 mL/min with UV detection at 246 nm. The calibration curves for the determination of all analytes showed good linearity over the investigated ranges (r > 0.999). The % relative standard deviation (% RSD) values were less than 0.34%, and the recoveries were between 95.79% and 99.94%. The values of luteolin-7-O-glucoside, salicin, myricetin, apigenin-3′-oxyethyl-7-O-glucoside, rutin, quercetin, luteolin, kaempferol, and apigenin were 1.0 μg g−1, 20.0 μg g−1, 32.9 μg g−1, 2.0 μg g−1, 29.5 μg g−1, 6.0 μg g−1, 1.0 μg g−1, 3.5 μg g−1, and apigenin was not found in the sample. This developed method can be used for evaluating the quality of different plant materials.

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Youzimai is a widespread wheat landrace and has been used extensively in breeding programs in China. In order to assess the genetic variation between and within Youzimai accessions, samples of 31 landrace accessions of wheat, all called ‘Youzimai’, were collected from 6 geographic regions in China and evaluated using morphological traits, seedling resistance to powdery mildew, gliadin and microsatellite markers. Typical differences among accessions were observed in morphological characteristics. Forty-five (58.4%) of 77 assayed SSR markers showed polymorphism over the entire collection and total 226 alleles were identified with an average of 5.02 alleles per locus. SSR data indicated that the accessions from Hebei province were the most diverse, as evidenced by greatest number of region-specific alleles and highest diversity index. These accessions, therefore, probably experienced the most substantial morphological and molecular evolution as a result of various natural and anthropomorphic influences. On the other hand, differentiation in gliadin phenotypes was found among seeds within 80.6% of total accessions and average 61.5% of entire collections showed heterogeneous and comprised resistant plants in reaction to powdery mildew, suggesting the presence of a wide diversity within the wheat landrace. By developing an intimate knowledge of the available wheat genotypes, appropriate selections can be made for commercial application in order to conserve and exploit the diversity of the wheat landraces.

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A reborn interest has occurred during the last decade toward wheat landraces for broadening genetic basis of modern wheat cultivars. The investigation of molecular traits within and between existing landraces of wheat can help scientists to develop appropriate strategies for their efficient maintenance and exploitation. The present study dealt with the gliadin characterization of forty-seven wheat landraces collected from wheat mainly planted areas of China, each of which was represented by a sample of at least 43 individuals. Twelve accessions selected on the basis of gliadin analysis were investigated further using 21 SSR markers. The results proved that landraces of wheat are a mixture of variable individuals genetically distinguishable from each other. Twelve of the analyzed 47 accessions were observed to be homogeneous, while 35 (74.5%) of them were heterogeneous in their gliadin composition. In total, 122 gliadin pattern were observed. On average, 10.1% (Gst) of the total variation arose from differentiation among regions, and 89.9% was attributed to within-region variation. Furthermore, nineteen of the 21 SSR markers were polymorphic across all the populations. The total number of the amplified DNA products was 110, with a mean of 6.11 alleles per locus. The values of genetic diversity within each landrace population varied from 0.006 to 0.351. Implications for the management of this valuable genetic resource are discussed.

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An allometric analysis of biomass and N mass allocation of rice (Oryza sativa L.) seedlings under non-shaded (100% of full sunlight) and shaded (30% of full sunlight) treatments were conducted. The allometric slopes and the intercepts were estimated using standardized major axis regression. Results indicated that biomass was preferentially allocated to stems during plant ontogeny, and leaves and roots were isometric when rice seedlings were not shaded. Under shade, however, more biomass was allocated to leaves and stems. N mass allocation was also altered by shading in that more N mass was allocated to the aerial shoots, and plants accumulated less N mass when shaded. Our study revealed that both biomass and N mass were in accordance with the optimal partitioning theory.

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A rapid and sensitive ultraperformance liquid chromatography-multiple reaction monitoring-multi-stage/mass spectrometry (UPLC-MRM-MS/MS) method has been developed for simultaneous quantification of salvianolic acid B and tanshinone IIA of salvia tropolone tablets in dog plasma. This was achieved by performing quantification using the MRM acquisition with two channels of MRM-MS/MS and MS full scan for more accuracy qualitative results, and the fragmentation transitions of m/z 295→249, 191 for tanshinone IIA and m/z 297→279, 251 for IS in positive mode, m/z 717→519, 321 for salvianolic acid B and m/z 295→267, 239 for IS in negative mode were selected. The UPLC separation was achieved within 3 min in a single UPLC run. Linear calibration curves were obtained over the concentration range of 10 pg/mL−1 ng/mL for tanshinone IIA and 100 pg/mL−1 for salvianolic acid B. Lower limit of quantitation (LLOQ) was 10 pg/mL and 100 pg/mL for tanshinone IIA and salvianolic acid B, respectively. The inter-day and intra-day precision (relative standard deviation, RSD) in all samples were less than 8.21%, and the recoveries were over 85.9% for both tanshinone IIA and salvianolic acid B. The two channels of MRM with MS full scan approach could provide both qualitative and quantitative results without the need for repetitive analyses and resulted in the reduction of further confirmation experiments and analytical time. The pharmacokinetic study of the two active components of salvia tropolone tablets following oral gavage administration of dogs was thus explored with this method.

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Hydrated goethite nanorodS

Vibration spectral properties, thermal stability, and their potential application in removing cadmium ions

Journal of Thermal Analysis and Calorimetry
Authors: X. Qiu, L. Lv, G. Li, W. Han, X. Wang, and L. Li

Abstract  

Vibration spectral properties and dehydration behaviors of goethite nanorods with diameters ranging from 13 to 32 nm were investigated using infrared spectroscopy, thermogravimetric analysis, and X-ray diffraction. All goethite nanorods were highly hydrated with physisorbed and chemisorbed water. As the diameters of goethite nanorods increased, the hydroxyl deformation vibration in the a-b plane showed a significant blue shift, while the Fe-O vibration in the a-b plane shifted to lower frequencies, indicating an enhancement of O-H bond and the ionicity of Fe-O in a-b plane. The hydrated goethite nanorods are also proved to be useful in environmental remedy because of their excellent removal ability of heavy metal ions.

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Abstract  

A brown and transparent ionic liquid (IL), [C4mim][FeCl4], was prepared by mixing anhydrous FeCl3 with 1-butyl-3-methylimidazolium chloride ([C4mim][Cl]), with molar ratio 1/1 under stirring in a glove box filled with dry argon. The molar enthalpies of solution, Δs H m, of [C4mim][FeCl4], in water with various molalities were determined by a solution-reaction isoperibol calorimeter at 298.15 K. Considering the hydrolyzation of anion [FeCl4] in dissolution process of the IL, a new method of determining the standard molar enthalpy of solution, Δs H m 0, was put forward on the bases of Pitzer solution theory of mixed electrolytes. The values of Δs H m 0 and the sum of Pitzer parameters:
\documentclass{aastex} \usepackage{amsbsy} \usepackage{amsfonts} \usepackage{amssymb} \usepackage{bm} \usepackage{mathrsfs} \usepackage{pifont} \usepackage{stmaryrd} \usepackage{textcomp} \usepackage{upgreek} \usepackage{portland,xspace} \usepackage{amsmath,amsxtra} \pagestyle{empty} \DeclareMathSizes{10}{9}{7}{6} \begin{document} $$(4\beta _{Fe,Cl}^{(0)L} + 4\beta _{C_4 mim,Cl}^{(0)L} + \Phi _{Fe,C_4 mim}^L )$$ \end{document}
and
\documentclass{aastex} \usepackage{amsbsy} \usepackage{amsfonts} \usepackage{amssymb} \usepackage{bm} \usepackage{mathrsfs} \usepackage{pifont} \usepackage{stmaryrd} \usepackage{textcomp} \usepackage{upgreek} \usepackage{portland,xspace} \usepackage{amsmath,amsxtra} \pagestyle{empty} \DeclareMathSizes{10}{9}{7}{6} \begin{document} $$(\beta _{Fe,Cl}^{(1)L} + \beta _{C_4 mim,Cl}^{(1)L} )$$ \end{document}
were obtained, respectively. In terms of thermodynamic cycle and the lattice energy of IL calculated by Glasser’s lattice energy theory of ILs, the dissociation enthalpy of anion [FeCl4], ΔH dis≈5650 kJ mol−1, for the reaction: [FeCl4](g)→Fe3+(g)+4Cl(g), was estimated. It is shown that large hydration enthalpies of ions have been compensated by large the dissociation enthalpy of [FeCl4] anion, Δd H m, in dissolution process of the IL.
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Abstract  

Treating iron-doped ZSM-5 zeolite with NO2 produced a complete change in the parameters of its 57Fe Mössbauer spectrum. The intensity of the absorption showed a dramatic decrease at 40–70 K with smooth, but anharmonic, behavior above this temperature. The results can be interpreted in terms of the modification of the iron environment to form an approximately square-well potential. This results in an asymmetric potential in which the iron becomes frozen in one region at low temperatures.

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Abstract

The enthalpies of mixing of six kinds of amino acid (glycine, L-alanine, L-valine, L-serine, L-threonine, and L-proline) with glycerol in aqueous solutions and the enthalpies of diluting of amino acid and glycerol aqueous solutions have been determined by flow microcalorimetry at 298.15 K. Employing McMillan–Mayer theory, the enthalpies of mixing and diluting have been used to calculate heterogeneous enthalpic pairwise interaction coefficients (h xy) between amino acids and glycerol in aqueous solutions. Combining h xy values of amino acids with glycol in the previous study, the variations of the h xy values between amino acids and glycerol have been interpreted from the point of view of solute–solute interactions.

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