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991.
以间苯三酚为起始原料,L-脯氨酸为催化剂,经由两步反应首次合成了Empetrifranzinans A(1a,总收率60%)和Empetrifranzinans C(总收率55%),其结构经1H NMR,13C NMR和HR-MS确证。初步药理筛选实验结果表明,1a对人结肠癌、肝癌、胃癌、肺腺癌、卵巢癌细胞表现出了较强的细胞毒作用,其IC50分别为<0.1,1.31,4.90,8.98和3.65μmol·L-1。 相似文献
992.
The determination of xenobiotics in keratinized matrices, such as nails and hair, has received considerable attention because of the relatively long detection window for compounds. The distribution of xenobiotics in fingernails, unlike hair, was equivocal. The main aim of this study was to use follow-up surveys to measure zolpidem profiles in nails after subjects consumed a single dose of the drug. In addition, the zolpidem concentrations in nails were compared with data for different biosamples, such as hair and blood from previous work. With these preconditions, a high-performance liquid chromatography–tandem mass spectrometry method was developed and validated for the determination of zolpidem in nails. Nails underwent alkaline hydrolysis and were extracted with diethyl ether. A Capcell Pak C18 MGII column was used to separate the target compound, and an API 4000 Qtrap mass spectrometer was used as a detector. The results for nail samples from seven subjects who had taken a single 10 mg zolpidem dose were significant: two relatively high zolpidem concentrations were observed in the long-term follow-up analysis of nails. The zolpidem concentration was less than 1.74 pg/mg and less than 3.29 pg/mg in fingernails and toenails, respectively. The subsequent peak concentration of zolpidem was observed between 10 and 15 weeks after each subject took a single dose of the drug. This result suggested that the germinal matrix area was a primary in vivo pathway for zolpidem secretion into the nail. The analysis of biosamples, such as nails, may be a useful adjunct to conventional methods of drug testing and hair analysis. Further research is needed concerning the contamination risk in analysis of nail biosamples. 相似文献
993.
Yue-Wei Zhang Hai-Yu Yan Ping Fu Fei Jiang Yao Zhang Wen-Xue Wu Jin-Xiang Li 《Analytical and bioanalytical chemistry》2013,405(16):5549-5555
The recognition of targets such as biomacromolecules, viruses and cells by their aptamers is crucial in aptamer-based biosensor platforms and research into protein function. However, it is difficult to evaluate the binding constant of aptamers and their targets that are hard to purify and quantify, especially when the targets are undefined. Therefore, we aimed to develop a modified capillary electrophoresis based method to determine the dissociation constant of aptamers whose targets are hard to quantify. A protein target, human thrombin, and one of its aptamers were used to validate our modified method. We demonstrated that the result calculated by our method, only depending on the aptamer’s concentrations, was consistent with the classical method, which depended on the concentrations of both the aptamers and the targets. Furthermore, a series of DNA aptamers binding with avian influenza virus H9N2 were confirmed by a four-round selection of capillary electrophoresis–systematic evolution of ligands by exponential enrichment, and we identified the binding constant of these aptamers by directly using the whole virus as the target with the modified method. In conclusion, our modified method was validated to study the interaction between the aptamer and its target, and it may also advance the evaluation of other receptor–ligand interactions. 相似文献
994.
995.
996.
Hui Hang Chunxiang Li Jianming Pan Linzi Li Jiangdong Dai Xiaohui Dai Ping Yu Yonghai Feng 《Journal of separation science》2013,36(19):3285-3294
Porous/magnetic molecularly imprinted polymers (PM‐MIPs) were prepared by Pickering emulsion polymerization. The reaction was carried out in an oil/water emulsion using magnetic halloysite nanotubes as the stabilizer instead of a toxic surfactant. In the oil phase, the imprinting process was conducted by radical polymerization of functional and cross‐linked monomers, and porogen chloroform generated steam under the high reaction temperature, which resulted in some pores decorated with easily accessible molecular binding sites within the as‐made PM‐MIPs. The characterization demonstrated that the PM‐MIPs were porous and magnetic inorganic–polymer composite microparticles with magnetic sensitivity (Ms = 0.7448 emu/g), thermal stability (below 473 K) and magnetic stability (over the pH range of 2.0–8.0). The PM‐MIPs were used as a sorbent for the selective binding of lambdacyhalothrin (LC) and rapidly separated under an external magnetic field. The Freundlich isotherm model gave a good fit to the experimental data. The adsorption kinetics of the PM‐MIPs was well described by pseudo‐second‐order kinetics, indicating that the chemical process could be the rate‐limiting step in the adsorption of LC. The selective recognition experiments exhibited the outstanding selective adsorption effect of the PM‐MIPs for target LC. Moreover, the PM‐MIPs regeneration without significant loss in adsorption capacity was demonstrated by at least four repeated cycles. 相似文献
997.
Jianing Mi Min Zhang Hongyang Zhang Yuerong Wang Shikun Wu Ping Hu 《Journal of separation science》2013,36(3):593-601
A high‐efficient and environmental‐friendly method for the preparation of ginsenosides from Radix Ginseng using the method of coupling of ultrasound‐assisted extraction with expanded bed adsorption is described. Based on the optimal extraction conditions screened by surface response methodology, ginsenosides were extracted and adsorbed, then eluted by the two‐step elution protocol. The comparison results between the coupling of ultrasound‐assisted extraction with expanded bed adsorption method and conventional method showed that the former was better than the latter in both process efficiency and greenness. The process efficiency and energy efficiency of the coupling of ultrasound‐assisted extraction with expanded bed adsorption method rapidly increased by 1.4‐fold and 18.5‐fold of the conventional method, while the environmental cost and CO2 emission of the conventional method were 12.9‐fold and 17.0‐fold of the new method. Furthermore, the theoretical model for the extraction of targets was derived. The results revealed that the theoretical model suitably described the process of preparing ginsenosides by the coupling of ultrasound‐assisted extraction with expanded bed adsorption system. 相似文献
998.
Ping Wang Hai tao Lv Ai hua Zhang Hui Sun Guang li Yan Ying Han Xiu hong Wu Xi jun Wang 《Journal of separation science》2013,36(21-22):3511-3516
999.
A new bridging ligand, 2,3‐di(2‐pyridyl)‐5‐phenylpyrazine (dpppzH), has been synthesized. This ligand was designed so that it could bind two metals through a NN‐CNN‐type coordination mode. The reaction of dpppzH with cis‐[(bpy)2RuCl2] (bpy=2,2′‐bipyridine) affords monoruthenium complex [(bpy)2Ru(dpppzH)]2+ ( 12+ ) in 64 % yield, in which dpppzH behaves as a NN bidentate ligand. The asymmetric biruthenium complex [(bpy)2Ru(dpppz)Ru(Mebip)]3+ ( 23+ ) was prepared from complex 12+ and [(Mebip)RuCl3] (Mebip=bis(N‐methylbenzimidazolyl)pyridine), in which one hydrogen atom on the phenyl ring of dpppzH is lost and the bridging ligand binds to the second ruthenium atom in a CNN tridentate fashion. In addition, the RuPt heterobimetallic complex [(bpy)2Ru(dpppz)Pt(C?CPh)]2+ ( 42+ ) has been prepared from complex 12+ , in which the bridging ligand binds to the platinum atom through a CNN binding mode. The electronic properties of these complexes have been probed by using electrochemical and spectroscopic techniques and studied by theoretical calculations. Complex 12+ is emissive at room temperature, with an emission λmax=695 nm. No emission was detected for complex 23+ at room temperature in MeCN, whereas complex 42+ displayed an emission at about 750 nm. The emission properties of these complexes are compared to those of previously reported Ru and RuPt bimetallic complexes with a related ligand, 2,3‐di(2‐pyridyl)‐5,6‐diphenylpyrazine. 相似文献
1000.
Yu‐Long Wang Meng Feng Xian Tao Qing‐Yun Tang Ying‐Zhong Shen 《Acta Crystallographica. Section C, Structural Chemistry》2013,69(1):25-28
The lanthanum(III) complexes tris(3,5‐diphenylpyrazolato‐κ2N,N′)tris(tetrahydrofuran‐κO)lanthanum(III) tetrahydrofuran monosolvate, [La(C15H11N2)3(C4H8O)3]·C4H8O, (I), and tris(3,5‐diphenyl‐1,2,4‐triazolato‐κ2N1,N2)tris(tetrahydrofuran‐κO)lanthanum(III), [La(C14H10N3)3(C4H8O)3], (II), both contain LaIII atoms coordinated by three heterocyclic ligands and three tetrahydrofuran ligands, but their coordination geometries differ. Complex (I) has a mer‐distorted octahedral geometry, while complex (II) has a fac‐distorted configuration. The difference in the coordination geometries and the existence of asymmetric La—N bonding in the two complexes is associated with intramolecular C—H...N/O interactions between the ligands. 相似文献