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Su R Wang X Xu X Wang Z Li D Zhao X Li X Zhang H Yu A 《Journal of chromatography. A》2011,1218(31):5047-5054
The multiwall carbon nanotubes (MWCNTs)-based matrix solid phase dispersion (MSPD) was applied for the extraction of hormones, including 17-α-ethinylestradiol, 17-α-estradiol, estriol, 17-β-estradiol, estrone, medroxyprogesterone, progesterone and norethisterone acetate in butter samples. The method includes MSPD extraction of the target analytes from butter samples, derivatization of hormones with heptafluorobutyric acid anhydride-acetonitrile mixture, and determination by gas chromatography-mass spectrometry. The mixture containing 0.30 g graphitized MWCNTs and 0.10 g MWCNTs was selected as absorbent. Ethyl acetate was used as elution solvent. The elution solvent volume and flow rate were 12 mL and 0.9 mL min(-1), respectively. The recoveries of hormones obtained by analyzing the five spiked butter samples were from 84.5 to 111.2% and relative standard deviations from 1.9 to 8.9%. Limits of detection and quantification for determining the analytes were in the range of 0.2-1.3 and 0.8-4.5 μg kg(-1), respectively. Compared with other traditional methods, the proposed method is simpler in the operation and shorter in the sample pretreatment time. 相似文献
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A novel hydrated cobalt tetraborate complex NH4[Co(NH3)5(H2O)][B4O5(OH)4]2·6H2O, was synthesized by the reaction of NH4‐borate aqueous with CoCl2 and its structure was determined by single crystal X‐ray diffraction. The crystal system of this complex is orthorhombic, the space group is Pnma, and the unit cell parameters are a=1.2901(2) nm, b=1.6817(3) nm, c=1.1368(2) nm, α=β=γ=90°, V=2.4742(8) nm3, and Z=4. This compound contains infinite borate layers constructed from [B4O5(OH)4]2? units via hydrogen bonds. The adjacent polyborate anion layers are further linked together with the octahedral [Co(NH3)5(H2O)]3+ groups through hydrogen bonds to form 3D framework. The groups and guest water molecules are deposited in the empty space of this framework and interact with the layers by extensive hydrogen bonds. Infrared and Raman spectra (4000–400 cm?1) of NH4[Co(NH3)5(H2O)][B4O5(OH)4]2·6H2O were recorded at room temperature and analyzed. Fundamental vibrational modes were identified and band assignments were made. The middle band observed at 575 cm?1 in Raman spectrum is the pulse vibration of [B4O5(OH)4]2?. 相似文献
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A novel peroxyoxalate chemiluminescence system has been designed for the determination of Triton X‐100 (TX‐100), in which a hydrophobic fluorescent conjugated polymer, poly[2,5‐bisnonyloxy‐1,4‐phenylene‐ethynylene‐9,10‐anthrylene] (PPEA) was employed as a fluorophor. A strong enhanced intensity of chemiluminescence (CL) was observed in the presence of TX‐100, due to the improved emission efficiency of PPEA in the presence of TX‐100. Under optimum conditions, the detection range of Triton X‐100 is between 1.0×10?7 and 1.0× 10?4 mol·L?1, with a detection limit at 6.0×10?8 mol·L?1. The relative standard deviation is 2.4% (n=6) for 1.0×10?6 mol·L?1 Triton X‐100. This method provides satisfying results in the detection of TX‐100 in nature water and biological samples with high sensitivity and wide linear range. 相似文献
955.
A novel ligand‐based pharmacophore model for KDR kinase was generated on the basis of chemical features of 30 KDR kinase inhibitors. This pharmacophore model consists of one hydrogen‐bond acceptor, one hydrogen‐bond donor and two hydrophobic groups. Several methods have been used to validate the model, suggesting that it can serve as a reliable tool for virtual screening to facilitate the discovery of novel KDR inhibitors. The model was then used as database search query from the National Cancer Institute (NCI) database for the rational design to identify new hit compound. 相似文献
956.
Colorectal cancer (CRC) is the third commonest malignancy cancer worldwide. Clear understandings of global metabolic profiling of the normal mucosa and cancer tissues are vitally important to aid optimizing the clinical management strategy and understanding CRC biology. We studied metabolic characteristics of 20 CRC and 20 distant normal mucosa tissues extracts from 20 patients using high resolution 1H NMR spectroscopy in conjunction with multivariate analyses, such as principal component analysis (PCA). Compared with distant normal mucosa tissues, lactate, taurine, ornithine and polyamine were present at significantly higher levels in CRC tissue extracts whereas myo‐inositol was present at significantly lower level. Two metabolites ratios such as myo‐inositol/taurine and myo‐inositol/(ornithine+polyamine) appear to be the most valuable biomarkers for the differentiation CRC from normal mucosa tissues. Our data suggested that HR 1H NMR spectroscopy combined with multivariate analyses is a potentially useful technology for detecting malignant changes in the normal mucosa tissues, the technique may be further exploited for future CRC biomarker research or identification of targets for therapeutic manipulations. 相似文献
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