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961.
962.
建立了加速溶剂萃取同步净化-同位素内标-气相色谱-高分辨质谱同时测定水产品中32种多氯联苯含量的方法。通过在加速溶剂萃取仪中加入2 g无水硫酸钠、1 g弗罗里硅土、50 g中性氧化铝作为吸附剂实现同步净化的效果,萃取溶剂为二氯甲烷-正己烷(1:1,v/v),萃取温度为100℃,循环2次。萃取结束后分别用0.5 mL浓硫酸净化两次,净化液浓缩定容后,采用气相色谱-高分辨质谱测定,同位素内标法定量。32种多氯联苯在0.1~20 μg/L范围内平均相对响应因子(RRF)的相对标准偏差(RSD)值(n=7)均小于15%,定量限(S/N=10)为0.3~1.9 ng/kg。在草鱼和海鲈鱼空白基质中做加标回收试验,添加水平为5、20和50 ng/kg,得到的平均回收率为71.9%~119.0%(n=6),RSD为3.5%~19.6%。该方法背景干扰低,灵敏度高,重现性好,回收率稳定,适用于水产品中多氯联苯的检测。 相似文献
963.
The title compound was synthesized by reaction of Cu(ClO4)2, picolinic acid and carbamide in C2H5OH/CH3CN solution, and characterized by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pbca with a=14.0481(8), b=9.0130(5), c=18.626(1)?, V=2358.3(2)?3, Z=4, Dx=1.771g·cm-3, μ=1.235mm-1 and F(000)=1276. The final R factor is 0.0440 for 1434 observed reflections. The X-ray analysis revealed that the copper(Ⅱ) atom is coordinated by two picolinic ligands in the equatorial plane, while the two oxygen atoms of perchlorate occupy the axial positions of octahedron with lengthened Cu-O distances, resulting in a 4+2 elongated octahedral environment. In the compound, there also exist two protonated carbamide cations for charge balance. CCDC: 195354. 相似文献
964.
Xiu Xia WANG Zhi Gang JIANG Yi Feng ZHANG 《中国化学快报》2006,17(1):125-128
Epoxy resins are widely used in coatings, adhesives and polymer composites, but the applications of cured epoxy resins are often restricted by their poor toughness. HBP can be used as toughener to improve the toughness of epoxy resins due to its high-dens… 相似文献
965.
966.
Various kinds of aluminum species in dealuminated mordenite were investigated in detail, and the quadrupole coupling constants
(QCCs) for aluminum atoms associated with these species were obtained by means of the newly introduced1H/27 AI TRAPWR method as well as27Al magic angle spinning (MAS) nuclear magnetic resonance (NMR). QCC values of 11.3, 15.3, 13.3 and (14.0± 0.6) MHz were determined
from the TRAPDOR profiles for Lewis acid sites, Bronsted acid sites (SiOHAl) and two kinds of non-framework aluminum species
Al(OH)
n
, respectively. The source of the “invisible Al” is discussed on the basis of the NMR experimental results. 相似文献
967.
Five new C19 diterpene alkaloids, leucanthumsines A ( 1 ), B ( 2 ), C ( 3 ), D ( 4 ), and E ( 5 ), were isolated from the Chinese medicinal herb Aconitum sungpanense var. leucanthum, together with the known C19 diterpene alkaloids pseudaconine, neoline, 1‐O‐methyldelphisine, crassicaudine, chasmanine, talatisamine, indaconitine, ezochansmanine, and leueantine D. The structures of these new alkaloids were elucidated by HR‐MS and advanced NMR methods, including 1H‐ and 13C‐NMR (DEPT), 1H,1H‐COSY, HMQC, and HMBC experiments. 相似文献
968.
High-speed counter-current chromatography was successfully applied for the first time to the isolation and purification of the bioactive carotenoid zeaxanthin from the cyanobacterium Microcystis aeruginosa. The crude zeaxanthin was obtained by extraction with organic solvents after the microalgal sample had been saponified. Preparative high-speed counter-current chromatography with a two-phase solvent system composed of n-hexane-ethyl acetate-ethanol-water (8:2:7:3, v/v/v/v) was successfully performed yielding zeaxanthin at 96.2% purity from 150 mg of the crude extract in a one-step separation. The recovery of zeaxanthin was 91.4%. This was also the first report that zeaxanthin was successfully separated and purified from microalgae. 相似文献
969.
A pyrene-functional fluoroionophore, 1 was used to construct a supramolecular 1/γ-CD complex for Cu2+ recognition in water. In aqueous γ-CD solution, 1 exhibits pyrene monomer fluorescence emission at 378 nm and 397 nm, while in the presence of Cu2+, it shows a pyrene excimer emission at 452 nm with a decrease in the monomer fluorescence due to the formation of a 1:2 metal-liganded complex. Based on the response characteristics of the supramolecular complex, a fluorescent ratiometric method was performed for the determination of Cu2+ concentration in water. With the optimum conditions described, Cu2+ in aqueous solution can be determined from 1.2 × 10−6 to 4.5 × 10−4 M. The Cu2+ selectivity of the complex is excellent, and the excimer fluorescence enhancements are very smaller induced by other heavy metal and transition metal ions. 相似文献
970.
Brownian dynamics (BD) and molecular dynamics (MD) simulations and electrostatic calculations were performed to study the binding process of kappa-PVIIA to the Shaker potassium channel and the structure of the resulting complex. BD simulations, guided by electrostatic interactions, led to an initial alignment between the toxin and the channel protein. MD simulations were then carried out to allow for rearrangements from this initial structure. After approximately 4 ns, a critical "induced fit" process was observed to last for approximately 2 ns. In this process, the interface was reorganized, and side chains were moved so that favorable atomic contacts were formed or strengthened, while unfavorable contacts were eliminated. The final complex structure was stabilized through electrostatic interactions with the positively charged side chain of Lys7 of kappa-PVIIA deeply inserted into the channel pore and other hydrogen bonds and by hydrophobic interactions involving Phe9 and Phe23 of the toxin. The validity of the predicted structure for the complex was assessed by calculating the effects of mutating charged and polar residues of both the toxin and the channel protein, with the calculated effects correlating reasonably well with experimental data. The present study suggests a general binding mechanism, whereby proteins are pre-aligned in their diffusional encounter by long-range electrostatic attraction, and nanosecond-scale rearrangements within the initial complex then lead to a specifically bound complex. 相似文献