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991.
992.
气相色谱-质谱法测定茶叶中的噻嗪酮残留量 总被引:6,自引:0,他引:6
建立了气相色谱-质谱法测定茶叶中噻嗪酮残留量的方法。茶叶中残留的噻嗪酮用丙酮-正己烷混合溶剂(1∶1)提取,提取液经Envi-Carb活性碳柱和LC-Alumina N中性氧化铝柱净化,浓缩定容后,直接用气相色谱-质谱进行分析和确证,外标法定量。以HP-5MS(30m×0.25mm i. d., 0.25 μm)石英毛细管柱为分离柱,噻嗪酮的分离效果良好。方法的线性范围为0.01~1.00μg/mL,检出限为0.01mg/kg,回收率为81.6%~97.2%,相对标准偏差为3.36%~5.78%。质谱监测离子选m/z为105、140、172、305amu,其强度比约为41∶13∶29∶17。样品前处理采用微量化学技术。 相似文献
993.
A method for preparative production of 3β,20S-dihydroxydammar-24-en-12-one 3,20-di-O-β-D-glucopyranoside (1), a glycoside from Panax japonicus, chikusetsusaponin-LT8 was developed. Chemical transformation of betulafolientriol, a component of Betula leaves extract, produced the 12-keto-20S-protopanaxadiol (3β,20S-dihydroxydammar-24-en-12-one) (2), exhaustive glycosylation of which by 2,3,4,6-tetra-O-acetyl-α-D-glucopyranosylbromide (3) under Koenigs—Knorr reaction conditions with subsequent removal of protecting groups formed 3β,20S-dihydroxydammar-24-en-12-one
3,20-di-O-β-D-glucopyranoside (1). The principal glycosylation product was 3β,20S-dihydroxydammar-24-en-12-one 3-O-β-D-glucopyranoside if equimolar amounts of (2) and (3) were used.
__________
Translated from Khimiya Prirodnykh Soedinenii, No. 1, pp. 44–48, January–February, 2006. 相似文献
995.
J. P. Doumerc J. M. Cocciantelli J. C. Grenier M. Pouchard P. Hagenmuller 《无机化学与普通化学杂志》1993,619(4):748-752
Magnetic susceptibility of V2O5 and of the α-, ?-, δ- and γ-LixV2O5 bronzes prepared either at high or at room temperature has been measured between liquid helium and ambient temperature. The results are representative of the localized character of the V4+ ion d-electron and, for high enough x-values, of the existence of antiferromagnetic interactions in a low dimensional system. The intrachain exchange integral J has been determined using the Bonner/Fischer model for Heisenberg chains with S = 1/2 spin. It is larger for the γ- than for the δ-phase. This result as well as the occurrence of long range ordering below TN ≈ 130 K in the γ-phase may be ascribed to ordering of V4+ and V5+ ions in the former bronze and to the random distribution of V4+ ions in the latter one. 相似文献
996.
997.
The basic theory of symplectic algorithm was introduced. A comparison between Runge-Kutta method and symplectic integration method was preformed in the simulation of the long time behavior of H + H2 system on BKMP potential energy surface. Our results reveal a dis-sipative behavior in the integral of ordinary differential equation by the fourth order Runge-Kutta method, which causes incorrect simulation results in QCT calculations. However, when the symplectic integration method is applied, the dissipative behavior is not found in the same system. When the initial state is the same, the energy deviation of fourth order symplectic integral method is almost one percent of that of fourth order Runge-Kutta method in a 60000-step simulation, and that of sixth order symplectic integral method is much less. These results show that the symplectic integral methods are always the better choice in the integral calculation of the long time behavior in maintaining energy conservation. 相似文献
998.
Wolfgang A. Herrmann Gerhard M. Lobmaier Martina Elison 《Journal of organometallic chemistry》1996,520(1-2):231-234
Oxometal complexes of molybdenum and tungsten in high oxidation states from stable adducts with 1,3-dimethylimidazoline-2-ylidene (L) 1. The first ‘carbene’ complexes of molybdenum(VI) [MoO2Cl(L)3]Cl (3a) and tungsten(VI) WO2Cl2(L)2 (4b) are reported. 相似文献
999.
B2O3/TiO2-ZrO2催化环己酮肟气相Beckmann重排反应研究Ⅱ.焙烧温度的影响 总被引:1,自引:0,他引:1
采用XRD、FT-IR和NH3-TPD等方法,研究了载体预焙烧温度和催化剂活化焙烧温度对B2O3/TIO2-ZRO2催化剂的结构、酸性和催化环己酮肟气相Beckmann重排反应性能的影响。结果表明,在383-773K范围内,载体预烧温度对催化剂性能的影响不大,但经973K高温预焙烧后,由于生成了ZrTiO4晶相,使其与H3BO3的相互作用减弱,从而导致催化剂的酸性和反应性能降低,提高催化剂活化焙烧温度,有利于B2O3与TiO2-ZrO2的相互作用,生成更多的Beckmann重排反应所需的中等强度酸中心,使催化剂的活性和选择性提高;但活化焙烧温度过高,会使催化剂中大量的B2O3晶粒析出,引起酸中心数量和催化活性的明显下降。 相似文献
1000.
[Co(amp)2Cl2]2[ZnCl4]体系中两对称异构体的2D NMR研究 总被引:7,自引:0,他引:7
The two symmetrical isomers in [Co(amp)2Cl2]2[ZnCl4](amp=2-(Aminomethyl)pyridine) system were syn-thesized by general oxidation method and were separated by chromatography and recrystallization method. Their configurations were assigned by using 2D NMR techniques, particularly the NOESY NMR spectra. Solvent used was Me2SO-d6 with the central peak of the CD3 septet as the reference ( 13C,δ 39.37; 1H,δ 2.49 relative to SiMe4). Cation exchange media used was Dowex 50Wx 2(H+ form, 200~400mesh; Biorad). 相似文献