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881.
A non-aqueous reversed phase HPLC was developed for determining alpha-tocopherol in Sea buckthorn oil capsule without the need for saponification. A reversed phase column (Alltima C(18), 4.6 x 250 mm, 5 microm) was used with a mobile phase of methanol-acetonitrile (95 : 5, v/v) and flow rate of 1 ml/min. The contents in capsule were extracted with n-hexane. Detection wavelength was set at 292 nm. Each analysis requires no longer than 20 min. The linearity range for alpha-tocopherol was 9.4-47.0 microg/ml. The detection limit was 0.94 microg/ml. The mean recovery was 95.82 (RSD 2.3%). This method is suitable for quantitative analysis of alpha-tocopherol in Sea buckthorn oil or its Traditional Chinese Medicinal preparation. 相似文献
882.
本文介绍水杨配合与4-氨基-3,5-二乙基-1,2,4-三唑缩合而成对称三唑Schif碱(SAETZ)与氯化铜(CuCl2)形成一种新的配合物Cu(SAETZ)2(SAETZ=4-(邻羟苯基亚甲基)-亚胺-3,5-二乙基-1,2,4-三唑)。配合物的晶体结构表明,分子中两个偶氮甲碱的N原子及两个酚氧原子与中心Cu原子形成规则的平面配位结构。晶体属单斜晶系,空间群P21/n,a=8.688(2),b=9.314(1),c=16.515(4),β=94.34(2)。,V=1332.5(7)3,Z=2。 相似文献
883.
Summary Three novel heterotrinuclear complexes have been prepared, [Cu2(oxdn)2Zn](ClO4)2 (1) and [Cu2(oxdn)2-M(H2O)2](ClO4)2 with M=Mn (2) and Co (3) [oxdn-oxamidobis (propionato)], and characterized by spectral data. The temperature dependence of the magnetic susceptibilities of (2) and (3) has been studied in the 4–300K range, and the exchange integrals J=–20.90cm–1 for (2) and J=–62.36cm–1 for (3) calculated. These results are commensurate with antiferromagnetic interactions between the adjacent metal ions. 相似文献
884.
Reduced Ni-Mo/Al(2)O(3) catalysts exhibit a behavior analogous to that of sulfided Ni-Mo/Al(2)O(3) catalysts in hydrogenation of linear aldehydes to alcohols. Similar to what has been previously reported for sulfided catalysts, NO and CO(2) can be used over the reduced Ni-Mo catalysts as probe molecules for the active sites responsible for two competing reactions -- aldehyde hydrogenation to alcohols and condensation reactions to heavy products, respectively. Reduced catalysts have a higher aldehyde conversion activity and alcohol selectivity than their sulfided counterparts. The reduction temperature has a strong effect on the surface density of anion vacancies, which are responsible for alcohol formation. Reduction temperature also plays a role in determining the abundance of OH groups on the alumina surface. The effect of reduction temperature also manifests itself through the differences seen in the oxidation states of Mo and Ni species. 相似文献
885.
Li-Ya Wang Xiao-Qiang Wang Kai Jiang Jiu-Li Chang Yu-Fang Wang 《Journal of Molecular Structure》2007,840(1-3):14-21
A new nitronyl nitroxide NIT2-bithph (1) and its manganese(II) compound [Mn(hfac)2(IMHBithph)]2·(NIT2-bithph)(C6H14) (2) (hfac = hexafluoroacetylacetonate; NIT2-bithph = 4,4,5,5-tetramethyl-2-(bithiophenal-2-yl)imidazoline-1-oxyl-3-oxide; IMHBithph = 1-hydroxy-2-bithiophenal-4,4,5,5-tetramethyl-4,5-dihydro- 1H-imidazole) have been synthesized and structurally characterized by X-ray diffraction methods. The units of compound 1 were connected as one-dimensional chain by the intermolecular hydrogen bonds which afford an intermolecular antiferromagnetic interaction between nitronyl nitroxide radicals within the chain (J = −1.89 cm−1). Compound 2 resulting from the reaction of Mn(hfac)2·2H2O and NIT2-bithph is dinuclear and includes the reduced amidino-oxide form of NIT2-bithph, it is made up of three parts: a [Mn(hfac)2(IMHBithph)]2 dimer unit, an uncoordinated NIT2-bithph radical and a noncoordinated solvent molecule of hexane, the molecule of radical is hydrogen bonded to its reduced form. Two reduced IMHBithph ligands bridge the two manganese(II) ions through their amidino-oxide oxygen atoms resulting in a small intramolecular antiferromagnetic interaction between the manganese ions (J = −1.55 cm−1). 相似文献
886.
Xi-Shang Sun Xing-Heng Wang Hai-Yan Tao Liang Wei Chun-Jiang Wang 《Chemical science》2020,11(40):10984
In this study, we developed an efficient Ir-catalyzed cascade umpolung allylation/2-aza-Cope rearrangement of tertiary α-trifluoromethyl α-amino acid derivatives for the preparation of a variety of quaternary α-trifluoromethyl α-amino acids in high yields with excellent enantioselectivities. The umpolung reactivity empowered by the activation of the key isatin-ketoimine moiety obviates the intractable enantioselectivity control in Pd-catalyzed asymmetric linear α-allylation. In combination with quasi parallel kinetic resolution or kinetic resolution, the generality of this method is further demonstrated by the first preparation of enantioenriched quaternary trifluoromethyl β-, γ-, δ- and ε-amino acid derivatives.In this study, we developed an efficient Ir-catalyzed cascade umpolung allylation/2-aza-Cope rearrangement for the preparation of a variety of quaternary trifluoromethyl α-ε-amino acids in high yields with excellent enantioselectivities. 相似文献
887.
The cold and heat denaturations of bovine P-lactoglobulin A ((β-lg A) has been studied in solutions of guanidine hydrochloride
(GuHCI) by differential scanning calorimetry (DSC). The experimental results are presented and discussed. It is shown that
the number of protons bound by the monomeric molecules of β-lg A was unchanged before and after its heat denaturation below
pH 3, and that the activation energy of the heat denaturation was depressed owing to the presence of GuHCI. In the solutions
with 2.50 and 3.06 mol/L of GuHCI, both the cold and heat denaturations of P-lg A were observed. In comparison with the heat
denaturation, the activation energy of cold denaturation was far lower and the number of GuHCl molecules bound by the unfolded
polypeptide chains after culd denaturation increased a lot. The absolute value of the enthalpy of cold denaturation was larger
than that of heat denaturation. It was found by the analysis that the contribution to the total denaturational enthalpy of
conformational change itself of the monomeric molecules of β-lg A was the lowest among the globulins, according to the average
of the number of heavy atoms.
Project supported by the National Natural Science Foundation of China, and by the fund for excellent items under Director
of the Institute of Chemistry. 相似文献
888.
Effects of double substitution on the thermodynamic stabilities of nitrogen radicals 总被引:1,自引:0,他引:1
Studiesonkineticsofradicalreactions[1]andonCHbonddissociationenergies(BDE)[2]haveshownthatcarbonradicalsarestabilizedbyeitheranelectrondonatinggroup(EDG)oranelectronwithdrawinggroup(EWG),andthatifacarbonradicalissubstitutedwithbothanEDGandanEWGatthesamecen… 相似文献
889.
6-Oxy-(N-succinimidyl acetate)-9-(2'-methoxycarbonyl)fluorescein (SAMF), a new fluorescein-based amine-reactive fluorescent probe was well designed, synthesized and used as a pre-column derivatizing reagent for the determination of aliphatic amines in HPLC. It exhibited relatively pH-independent fluorescence (pH 4-9) and excellent photostability. The derivatization was performed at room temperature in 6min. On a C18 column, the derivatives of SAMF with eight aliphatic amines were baseline separated in 28 min with a mobile phase of methanol-water (57:43, v/v) containing 10 mmol l(-1) pH 5.0, H3Cit3-NaOH buffer. With fluorescent detection at lambda(ex)/lambda(em) = 484/516 nm, the detection limit could reach 2-320 fmol (signal-to-noise = 3), which was equivalent to or better than the detection limits obtained from other analytical methods of aliphatic amines. The proposed method has been applied to the determination of the aliphatic amines in environmental and food samples such as lake water, red wine, white wine, and cheese with satisfying recoveries varying from 95 to 106%. 相似文献
890.
The synthesis of a fluorous diol 4 bearing a perfluorodecyl chain was described. A series of boronic acid were attached to 4 by esterification. The purification of the products was fulfilled by facile filtration instead of expensive and environmental troublesome fluorous liquid-liquid extraction. The Suzuki cross-coupling reactions of the formed fluorous boronates 5 underwent smoothly and the fluorous diol 4 was recycled in good yields. 相似文献