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  • Author or Editor: X. Yang x
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Summary

The method of high-performance liquid chromatography (HPLC) with diode array detector (DAD) was used and validated for the simultaneous determination of nine flavonoids (rutin, myricetin, quercitrin, quercetin, luteolin, genistein, kaempferol, apigenin, and isorhamnetin) in beagle dog plasma. Plasma sample was pre-treated with acetonitrile (containing 0.05% formic acid). Chromatographic separation was performed on a kromasil C18 column (250 × 4.6 mm, 5 µm) maintained at 35 °C. The mobile phase was a mixture of methanol and 0.2% formic acid with a step linear gradient. At 1.0 mL min−1 flow rate, the eluent of other eight flavonoids was detected simultaneously at 360 nm with good separation except genistein (detected at 254 nm). Under optimum conditions, the correlation coefficient between the peak area and the concentrations for each analyte was all above 0.999. The intra-day and inter-day precisions were less than 10% for all analytes. The limit of detection and the limit of quantification for the selected nine flavonoids were 0.006–0.03 and 0.02–0.12 g mL−1, respectively. The extracted recoveries of selected nine flavonoids were 74.02%–99.37%. The assay has been successfully applied to determine concentrations of nine flavonoids in plasma from beagle dog after being intravenously administrated Ginkgo biloba extract.

Open access

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.

Open access

Abstract  

Supramolecular 2,3- and 2,5-pyridinedicarboxylate (PDC) intercalated ZnAl-layered double hydroxides (2,3- and 2,5-PDC–ZnAl–LDHs) have been prepared by ion exchange method. The structure and composition of the intercalated materials have been studied by X-ray diffraction (XRD) and inductively coupled plasma emission spectroscopy (ICP). The study indicates that the 2,3-PDC and 2,5-PDC anions are accommodated as interdigitated bilayer and monolayer arrangement respectively between the sheets of LDHs. Furthermore, their thermal decomposition processes were studied by the use of in situ high temperature X-ray diffraction (HT-XRD), and the combined technique of thermogravimetry-differential thermal analysis-mass spectrometry (TG-DTA-MS) under N2 atmosphere. Based on the comparison study on the temperatures of both decarboxylation and complete decomposition of interlayer PDC, it can be concluded that 2,5-PDC–ZnAl–LDHs has higher thermal stability than that of 2,3-PDC–ZnAl–LDHs.

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Abstract  

Solid complexes of M(His)2Cl2 nH2O (M=Mn, Co, Ni, Cu) of MnCl26H2O, CoCl26H2O, NiCl26H2O, CuCl22H2O and L-α-histidine (His) have been prepared in 95% ethanol solution and characterized by elemental analyses, chemical analyses, IR and TG-DTG. The constant-volume combustion energies of the complexes have been determined by a rotating-bomb calorimeter. And the standard enthalpies of formation of the complexes have been calculated as well.

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Abstract  

The solid complexes of Cr(NO3)3 with L-α-amino acids (AA=Val, Leu, Thr, Arg, Phe and Try) have been prepared in 95% alcoholic, the compositions of which were identified as the general formula Cr(AA)2(NO3)32H2O by elemental and chemical analyses. The bonding characteristics of the title complexes were characterized by IR, indicating that nitrogen and oxygen atoms in the ligands coordinated to Cr3+ in a bidentate fashion. With the aid of TG-DTG and IR techniques, the complexes were subjected to thermal decomposition in an atmosphere of oxygen, presuming that the decompositions of the complexes consist of two steps and the complexes were decomposed into chromium hemitrioxide after undergoing dehydration and skeleton splitting of the complexes. The constant volume energies of combustion of the complexes were determined by a RBC-P type rotating-bomb calorimeter. According to Hess's law, the standard enthalpies of formation of the complexes were calculated as (-1831.404.40), (-2542.036.13), (-1723.813.99), (-2224.313.02), (-2911.616.53) and (-659.327.42) kJ mol-1, respectively.

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Summary  

Cyanocobalamin (CNCbl), a kind of vitamin B12 (cobalamin, Cbl), which has a special binding capability to rapid dividing cells and proliferating tissue, especially tumors, has been modified and labeled by 99mTc. The optimal labeling condition was determined, and the biodistribution of 99mTc-DTPA-b-CNCbl both in normal mice and TA2 mice bearing MA891 mammary tumors were studied. 99mTc-DTPA-b-CNCbl showed low uptake and rapid clearance in nontarget tissues, and renal excretion. About 40% of uptake at 1 hour remained in the tumor at 12 hours p.i. The satisfying ratio of T/NT was acquired at 6 hours p.i.

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Genotypes with various Vp-1B alleles perform different levels of pre-harvest sprouting (PHS) tolerance. In this study, 217 white-grained wheat cultivars, including 75 landraces, 39 historical cultivars, and 103 modern cultivars from five major regions of China, were examined to characterize the diversity of the Viviparous-1B ( Vp-1B ) locus associated with PHS tolerance. Four Vp-1B alleles were identified, three ( Vp-1Ba , Vp-1Bb and Vp-1Bc ) of which were previously reported in Chinese wheat cultivars. A new allele, Vp-1Be , was identified in the PHS tolerant landrace Hongheshangtou. Sequence analysis showed that Vp-1Be had an insertion of a 4-bp fragment, two SNPs, and a deletion of an 83-bp fragment compared with the nucleotide sequence of Vp-1Ba (AJ400713), all located in the third intron. Vp-1Be shared 97.80% similarity with the nucleotide sequence of AJ400713. The frequencies of Vp-1Ba , Vp-1Bb , and Vp-1Bc were 36.0%, 5.3%, and 57.3% in landraces; 23.1%, 7.7%, and 69.2% in historical cultivars; and 52.4%, 0%, and 47.6% in current cultivars, respectively.

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Stripe rust, caused by Puccinia striiformis f. sp. tritici, was one of the most disaster foliar diseases for wheat-growing areas of the world. Thinopyrum intermedium has provided novel resistance genes to multi-fungal disease, and new wheat-Th. intermedium derivatives for stripe rust resistance still need to develop for wheat breeding. Wheat line X484-3 was selected from a cross between wheat line MY11 and wheat-Th. intermedium ssp. trichophorum partial amphiploid TE-1508, and was characterized by genomic in situ hybridization (GISH) and functional molecular markers. Chromosome counting revealed that the X484-3 was 2n = 44 and GISH analysis using Pseudoroegneria spicata genomic DNAas a probe demonstrated that X484-3 contained a pair of St-chromosomes from Th. intermedium donor parents. The functional molecular markers confirmed that introduced St-chromosomes belonging to linkage group 7, indicating that line X484-3 was a 7St addition line. The resistance observation displayed that the introduced Th. intermedium ssp. trichophorum derived chromosomes 7St were responsible for the stripe rust resistances at adult plant. The identified wheat-Th. intermedium chromosome 7St addition line X484-3 can be used as a donor in wheat breeding for stripe rust resistance.

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An efficient and sensitive analytical method based on precolumn derivatization and gas chromatography—mass spectrometry—selected ion monitoring (GC—MS—SIM) was proposed and validated for analysis of two cembrenediols (CBDs) which are α-cembrenediol and β-cembrenediol in tobacco samples. CBDs in tobacco samples were extracted by sonication with 50 mL dichloromethane for 10 min before derivatized with 2:3 (v/v) bis(trimethylsilyl)trifluoroacetamide (BSTFA)—pyridine at 20 °C for 100 min. CBDs’ level in tobacco samples was analyzed by GC—MS—SIM and quantified by the internal standard method. The linear range for α-CBD and β-CBD was 13.6–554.6 μg mL−1 and 4.11–162.6 μg mL−1, and the correlation coefficients of both were 0.9998. The limit of detection (LOD) and limit of quantification (LOQ) of α-cembrenediol and β-cembrenediol were 0.40 μg g−1 and 1.34 μg g−1, and 0.27 μg g−1 and 0.90 μg g−1, respectively. Average recoveries of α-CBD and β-CBD were 94.4–99.9% and 91.9–98.2% while the relative standard deviations (RSDs, n = 5) were ranged from 2.67 to 5.6% and 2.04 to 4.22%, respectively. This proposed analytical method has been successfully applied to analyze CBDs in tobacco samples.

Open access

Protein and starch are important in wheat quality and yield. To understand the genetic relationship between protein and starch at the quantitative trait locus (QTL)/gene level, 168 doubled haploid (DH) lines were used at three locations over 2 years. The QTLs for proteinfraction contents and starch content were analyzed by unconditional and conditional QTL mapping. We detected 17 unconditional additive QTLs (four albumin QTLs, three globulin QTLs, six gliadin QTLs, four glutenin QTLs) controlling protein-fraction contents. We detected 19 conditional QTLs (five albumin QTLs, three globulin QTLs, five gliadin QTLs, six glutenin QTLs) based on starch content. Of these QTLs, QAlu1B, QGlo6A, QGli1B, QGli7A, QGlu1B and QGlu1D increased the protein-fraction contents independent of the starch content. These QTLs could regulate the usual inverse relationship between protein and starch in wheat seeds. The results could possibly be used in the simultaneous improvement of grain protein and starch content in wheat breeding.

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