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Abstract  

The power-time curves of Tetrahymena thermophila exposed to tributyltin (TBT) were detected by microcalorimetry. Metabolic rate (r) decreased significantly while peak time (PT) increased with the enhancement of TBT level. Compared with the measured multibiomarker including catalase, lactate dehydrogenase, glutathione S-transferase, ATPase and membrane fluidity, PT and r could be sensitive biomarkers for assessing TBT toxicity at cellular level. The effective concentrations obtained by them were consistent to those obtained by the protozoan community toxicity test. As a result, the microcalorimetric assay of T. thermophila had a great potential in assessing TBT acute toxicity and monitoring TBT pollution in the freshwater ecosystem.

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Abstract  

Two compounds of antimony trichloride and bismuth trichloride with valine are synthesized by solid phase synthesis at room temperature. Their compositions, determined by element analysis, are Sb(C5H10O2N)3·2H2O and Bi(C5H10O2N)2Cl·0.5H2O. The crystal structure of antimony complex with valine belongs to triclinic system and its lattice parameters are: a=0.9599 nm, b=1.5068 nm, c=1.9851 nm, α=92.270, β=95.050, γ=104.270. The crystal structure of bismuth complex with valine belongs to monoclinic system and its lattice parameters are: a=1.6012 nm, b=1.8941 nm, c=1.839 nm, β=99.73°. The far-infrared spectra and infrared spectra show that the amino group and carboxyl of valine may be coordinated to antimony and bismuth, respectively, in two compounds. The TG-DSC results also reveal that the complexes were formed.

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This study aims to develop and validate a high-performance size-exclusion chromatography (HPSEC) method to determine the amount of polymer in cefmetazole sodium for injection and to compare this method with gel chromatography. A Zenix SEC-150 column was used with the mobile phase of phosphate buffer solution (pH 7.0; 0.01 M)—acetonitrile (90:10 v/v) at a flow rate of 0.8 mL min−1 and a detection wavelength of 240 nm. The polymer was quantified by an external standard method with self-control, and the amount was expressed by the percentage of cefmetazole. The HPSEC method was validated for specificity, linearity, and precision. The chromatographic conditions, chromatographic performances, sensitivity, linearity, and precision of the developed HPSEC method and gel chromatography were compared, and both methods were subsequently used to determine the amount of polymer from seven batches of samples. The HPSEC method was fully validated. The time of isocratic elution for sample assay was less than 14 min. The results of comparison indicate that the developed HPSEC method was superior to gel chromatography. The Student t test results also showed significant difference in the amount of polymer from the samples obtained by the two methods. Thus, the HPSEC method with two obvious advantages, the superior sensitivity and a shorter analysis time, is more suitable for determination of polymer amount in cefmetazole sodium for injection to control the quality of the product.

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Abstract

High-performance liquid chromatography with a hydrophilic-interaction liquid chromatographic (HILIC) column has been successfully used to retain and separate the polar phosphonic herbicides glyphosate and glufosinate. Online electrospray tandem ion-trap mass spectrometric and DAD detection were used. The effects on the separation of mobile phase acetonitrile content, buffer concentration, and flow rate, and of column temperature, were investigated. With UV-visible detection at 195 nm, LOQ were <850 mg kg−1, showing the method is suitable for product quality control of these herbicides alone or in combination. Tandem mass spectrometric conditions were optimized for ion-trap detection. Quantification was by use of selected reaction monitoring transitions m/z 168 → 150 in negative-ion mode for glyphosate and m/z 182 → 136 in positive-ion mode for glufosinate. Limits of detection (LOD; S/N > 3) were 0.20 and 0.16 ng for glyphosate and glufosinate, respectively, and the respective limits of quantification (LOQ; S/N = 10) were 0.02 and 0.05 mg kg−1. Sample derivatization was not necessary to achieve low detection limits in residue analysis in this study. Recovery from watermelon, spinach, potato, tomato, radish-root, and water fortified with the herbicides ranged from 63.6 to 107.3% and relative standard deviations were <15.3%.

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Summary

A rapid and sensitive method for the identification and quantification of yohimbine in Pausinystalia yohimbe is described. The method used is liquid chromatography-quadrupole ion trap mass spectrometry (LC-QIT/MS). The yohimbine standard solution was directly infused into the ion trap mass spectrometers (IT/MS) for collecting the MSn spectra. The major fragment ions of yohimbine were confirmed by MSn at m/z 355, 224, 212, and 144, in the positive-ion mode. The possible main fragment ion cleavage pathway was studied. Yohimbine provided good signals corresponding to the protonated molecular ion [M + H]+. The method is reliable and reproducible, and the detection limit is 0.1 ng mL-1. The method was validated in the concentration range 0.1–50 μg mL−1; the intra- and interday precision ranged from 1.36% to 2.73% and the accuracy was 96.5–108.2%. The mean recovery of yohimbine was 97.1–101% with a relative standard deviation (RSD) <1.93%. The LC-IT/MS method was successfully applied to determine the yohimbine in P. yohimbe.

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Abstract  

Research on extracted 90Y with di(2-ethylhexyl) orthophosphoric acid (P204) in lipiodol for liver cancer was made to evaluate the stability of extracted 90Y with P204 in lipiodol (90Y-P204-lipiodol) in serum of newly-born cattle and human’s blood. At first, P204 (extractant) was dissolved in lipiodol (organic phase). Secondly, 90Y was extracted to organic phase after adding 90Y solution into test tube with P204 and lipiodol in it. The extracting efficiency with 0.01 mol/l P204 could reach 99.4%. The stability of 90Y-P204-lipiodol has been experimented in physiological saline solution as preparation for further stability experiment. The result indicated that the extracted 90Y lost 0.02%–0.36% in physiological saline solution. The results of further stability experiment showed that loss efficiencies of extracted 90Y after adding newly-born cattle serum 1 hour, 1 day, 3 and 7 days are 3.38%, 3.12%, 4.29% and 6.62%, respectively, and loss efficiencies of extracted 90Y after adding human’s blood 1 hour, 1 day, 3 and 7 days are 2.55%, 5.91%, 7.88% and 5.63%, respectively. Our data also indicated that 90Y is the most possible radioisotope for being extracted with P204 in lipiodol to treat hepatocellular carcinoma, particularly in cases of unresectable liver tumors, since 90Y is available from several commercial sources in clinical quality. We conclude that the stability of 90Y-P204-lipiodol tested with newly-born cattle serum and human’s blood attained great results. 90Y-P204-lipiodol is a kind of potential and exciting pharmaceutical in inerventional therapy for liver cancer and we can carry on the further animal test and clinical trial.

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Aegilops sharonensis (Sharon goatgrass) is a valuable source of novel high molecular weight glutenin subunits, resistance to wheat rust, powdery mildew, and insect pests. In this study, we successfully hybridized Ae. sharonensis as the pollen parent to common wheat and obtained backcross derivatives. F1 intergeneric hybrids were verified using morphological observation and cytological and molecular analyses. The phenotypes of the hybrid plants were intermediate between Ae. sharonensis and common wheat. Observations of mitosis in root tip cells and meiosis in pollen mother cells revealed that the F1 hybrids possessed 28 chromosomes. Chromosome pairing at metaphase I of the pollen mother cells in the F1 hybrid plants was low, and the meiotic configuration was 25.94 I + 1.03 II (rod). Two pairs of primers were screened out from 150 simple sequence repeat markers, and primer WMC634 was used to identified the presence of the genome of Ae. sharonensis. Sequencing results showed that the F1 hybrids contained the Ssh genome of Ae. sharonensis. The sodium dodecyl sulfate polyacrylamide gel electrophoresis profile showed that the alien high molecular weight glutenin subunits of Ae. sharonensis were transferred into the F1 and backcross derivatives. The new wheat-Ae. sharonensis derivatives that we have produced will be valuable for increasing resistance to various diseases of wheat and for improving the quality of bread wheat.

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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.

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To study the development of starch granules in polyploid wheats, we investigated the expression of starch synthetic genes between the synthetic hexaploid wheat SHW-L1, its parents T. turgidum AS2255 and diploid Ae. tauschii AS60. The synthetic hexaploid wheat SHW-L1 showed significantly higher starch content and grain weight than its parents. Scanning electron microscopy (SEM) showed that SHW-L1 rapidly developed starch granules than AS2255 and AS60. The amount of B-type granule in AS60 was less than that in SHW-L1 and AS2255. RT-qPCR result showed that the starch synthetic genes AGPLSU1, AGPLSU2, AGPSSU1, AGPSSU2, GBSSI, SSIII, PHO1 and PHO2 expressed at earlier stages with larger quantity in SHW-L1 than in its parents during wheat grain development. The expression of the above mentioned genes in AS60 was slower than in SHW-L1 and AS2255. The expression pattern of starch synthase genes was also associated with the grain weight and starch content in all three genotypes. The results suggested that the synthetic hexaploid wheat inherited the pattern of starch granule development and starch synthase gene expression from tetraploid parent. The results suggest that tetraploid wheat could plays more important role for starch quality improvement in hexaploid wheat.

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Cereal Research Communications
Authors: S. Wang, D. Chen, G. Guo, T. Zhang, S. Jiang, X. Shen, D. Perovic, S. Prodanovic, and Y. Yan

In this work, 9 novel LMW-GS genes (6 LMW-m and 3 LMW-i type) from 4 diploid and 1 tetraploid Aegilops species were amplified and cloned by allelic-specific PCR. Analysis of the deduced amino acid sequences showed that 7 and 2 LMW-GS had 9 and 7 cysteines, respectively. Four LMW-m type subunits genes had an extra cysteine at the C-terminal III, which could form intermolecular disulphide bonds to extend the chains, and therefore would facilitate to form larger gluten polymers. This suggested that these genes are expected to be used as candidate genes for wheat quality improvement. The correlation between specific N-terminal sequences and a decapeptide deletion in the C-terminal II in LMW-GS encoded by D genome was found. Particularly, if LMW-GS possessed a METRCIPG-N-terminal beginning sequences and a decapeptide (LGQCSFQQPQ) deletion in the C-terminal II, they could be encoded by D genome.

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